# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C114 H190 B2 Fe2 P6, C4 H16 O' _chemical_formula_sum 'C118 H206 B2 Fe2 O P6' _chemical_formula_weight 1959.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3106(8) _cell_length_b 21.7915(7) _cell_length_c 22.8536(7) _cell_angle_alpha 90.00 _cell_angle_beta 126.5720(10) _cell_angle_gamma 90.00 _cell_volume 11323.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7177 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.16 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4296 _exptl_absorpt_coefficient_mu 0.388 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8007 _exptl_absorpt_correction_T_max 0.8828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 3 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41539 _diffrn_reflns_av_R_equivalents 0.1119 _diffrn_reflns_av_sigmaI/netI 0.1295 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.08 _reflns_number_total 11211 _reflns_number_gt 7001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was highly disordered, and the dataset was modelled with the use of free variables and appropriate restraints. The dataset was not strong enough to permit for location of all of the disordered atoms, resulting in some large U-values. The dataset is 99.7 % complete to theta = 25.24. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11211 _refine_ls_number_parameters 722 _refine_ls_number_restraints 1152 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.997 _refine_ls_restrained_S_all 1.921 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.59144(3) 0.12056(3) 0.04583(4) 0.0162(2) Uani 1 1 d U A . P1 P 0.63574(6) 0.11111(7) 0.16669(8) 0.0183(4) Uani 1 1 d U . . P2 P 0.58310(6) 0.22201(6) 0.05120(8) 0.0174(4) Uani 1 1 d U . . P3 P 0.67975(6) 0.13607(6) 0.06911(8) 0.0185(4) Uani 1 1 d U . . B1 B 0.7046(3) 0.2215(3) 0.1847(3) 0.0192(15) Uani 1 1 d U . . C1 C 0.7562(2) 0.2651(2) 0.2519(3) 0.0196(13) Uani 1 1 d U A . C2 C 0.8149(2) 0.2476(3) 0.2959(3) 0.0251(14) Uani 1 1 d U . . H2 H 0.8259 0.2112 0.2840 0.030 Uiso 1 1 calc R A . C3 C 0.8579(2) 0.2806(3) 0.3561(3) 0.0297(15) Uani 1 1 d U A . H3 H 0.8973 0.2660 0.3853 0.036 Uiso 1 1 calc R . . C4 C 0.8441(3) 0.3356(3) 0.3748(3) 0.0293(15) Uani 1 1 d U . . H4 H 0.8737 0.3600 0.4145 0.035 Uiso 1 1 calc R A . C5 C 0.7865(3) 0.3525(3) 0.3333(3) 0.0387(17) Uani 1 1 d U A . H5 H 0.7753 0.3882 0.3463 0.046 Uiso 1 1 calc R . . C6 C 0.7443(3) 0.3195(3) 0.2735(3) 0.0341(16) Uani 1 1 d U . . H6 H 0.7049 0.3341 0.2453 0.041 Uiso 1 1 calc R A . C7 C 0.6792(2) 0.1776(2) 0.2198(3) 0.0191(13) Uani 1 1 d U A . H7A H 0.6549 0.2035 0.2278 0.023 Uiso 1 1 calc R . . H7B H 0.7132 0.1630 0.2681 0.023 Uiso 1 1 calc R . . C8 C 0.6501(2) 0.2634(2) 0.1172(3) 0.0199(13) Uani 1 1 d U A . H8A H 0.6641 0.2834 0.0913 0.024 Uiso 1 1 calc R . . H8B H 0.6406 0.2963 0.1386 0.024 Uiso 1 1 calc R . . C9 C 0.7327(2) 0.1773(2) 0.1541(3) 0.0169(13) Uani 1 1 d U A . H9A H 0.7587 0.1468 0.1923 0.020 Uiso 1 1 calc R . . H9B H 0.7576 0.2031 0.1468 0.020 Uiso 1 1 calc R . . C1_1 C 0.6838(3) 0.0431(3) 0.2051(3) 0.0402(18) Uani 1 1 d U A . H1A_1 H 0.6579 0.0066 0.1854 0.048 Uiso 1 1 calc R . . H1B_1 H 0.7066 0.0423 0.1849 0.048 Uiso 1 1 calc R . . C2_1 C 0.72842(14) 0.03376(18) 0.28860(19) 0.0214(14) Uani 1 1 d DU . . H2_1 H 0.7144 0.0579 0.3128 0.026 Uiso 1 1 calc R A . C3_1 C 0.78984(17) 0.05590(18) 0.3182(2) 0.0315(16) Uani 1 1 d DU A . H3A_1 H 0.7884 0.1003 0.3079 0.038 Uiso 1 1 calc R . . H3B_1 H 0.8036 0.0339 0.2930 0.038 Uiso 1 1 calc R . . C4_1 C 0.83342(16) 0.04506(19) 0.4004(2) 0.0407(18) Uani 1 1 d DU . . H4A_1 H 0.8734 0.0571 0.4172 0.049 Uiso 1 1 calc R A . H4B_1 H 0.8225 0.0709 0.4262 0.049 Uiso 1 1 calc R . . C5_1 C 0.83345(16) -0.0219(2) 0.4184(2) 0.0464(19) Uani 1 1 d DU A . H5A_1 H 0.8496 -0.0469 0.3979 0.056 Uiso 1 1 calc R . . H5B_1 H 0.8596 -0.0272 0.4720 0.056 Uiso 1 1 calc R . . C6_1 C 0.7731(2) -0.04507(19) 0.3890(2) 0.0424(18) Uani 1 1 d DU . . H6A_1 H 0.7588 -0.0241 0.4142 0.051 Uiso 1 1 calc R A . H6B_1 H 0.7750 -0.0896 0.3987 0.051 Uiso 1 1 calc R . . C7_1 C 0.73012(16) -0.03354(18) 0.3072(2) 0.0401(18) Uani 1 1 d DU A . H7A_1 H 0.7419 -0.0585 0.2816 0.048 Uiso 1 1 calc R . . H7B_1 H 0.6903 -0.0468 0.2898 0.048 Uiso 1 1 calc R . . C1_2 C 0.5819(9) 0.0979(12) 0.1922(11) 0.004(4) Uani 0.478(5) 1 d PU A 1 H1A_2 H 0.5596 0.1366 0.1805 0.005 Uiso 0.478(5) 1 calc PR A 1 H1B_2 H 0.5533 0.0667 0.1578 0.005 Uiso 0.478(5) 1 calc PR A 1 C2_2 C 0.6012(3) 0.0787(4) 0.2675(3) 0.016(3) Uani 0.478(5) 1 d PDU A 1 H2_2 H 0.6286 0.0430 0.2848 0.019 Uiso 0.478(5) 1 calc PR A 1 C3_2 C 0.5463(2) 0.0596(3) 0.2604(3) 0.018(3) Uani 0.478(5) 1 d PDU A 1 H3A_2 H 0.5279 0.0241 0.2270 0.021 Uiso 0.478(5) 1 calc PR A 1 H3B_2 H 0.5176 0.0938 0.2390 0.021 Uiso 0.478(5) 1 calc PR A 1 C4_2 C 0.5605(3) 0.0423(3) 0.3342(4) 0.029(3) Uani 0.478(5) 1 d PDU A 1 H4A_2 H 0.5235 0.0332 0.3282 0.035 Uiso 0.478(5) 1 calc PR A 1 H4B_2 H 0.5852 0.0048 0.3530 0.035 Uiso 0.478(5) 1 calc PR A 1 C5_2 C 0.5927(3) 0.0941(4) 0.3885(3) 0.023(3) Uani 0.478(5) 1 d PDU A 1 H5A_2 H 0.5657 0.1295 0.3727 0.027 Uiso 0.478(5) 1 calc PR A 1 H5B_2 H 0.6041 0.0806 0.4367 0.027 Uiso 0.478(5) 1 calc PR A 1 C6_2 C 0.6468(3) 0.1142(4) 0.3959(3) 0.027(3) Uani 0.478(5) 1 d PDU A 1 H6A_2 H 0.6761 0.0807 0.4178 0.033 Uiso 0.478(5) 1 calc PR A 1 H6B_2 H 0.6643 0.1502 0.4287 0.033 Uiso 0.478(5) 1 calc PR A 1 C7_2 C 0.6319(3) 0.1311(3) 0.3218(4) 0.026(3) Uani 0.478(5) 1 d PDU A 1 H7A_2 H 0.6061 0.1677 0.3025 0.032 Uiso 0.478(5) 1 calc PR A 1 H7B_2 H 0.6685 0.1417 0.3277 0.032 Uiso 0.478(5) 1 calc PR A 1 C1_21 C 0.5944(9) 0.0949(13) 0.2003(13) 0.036(7) Uani 0.522(5) 1 d PU A 2 H1A_21 H 0.5560 0.1160 0.1679 0.043 Uiso 0.522(5) 1 calc PR A 2 H1B_21 H 0.5861 0.0503 0.1943 0.043 Uiso 0.522(5) 1 calc PR A 2 C2_21 C 0.6201(3) 0.1121(3) 0.2822(3) 0.019(3) Uani 0.522(5) 1 d PDU A 2 H2_21 H 0.6620 0.1249 0.3077 0.022 Uiso 0.522(5) 1 calc PR A 2 C3_21 C 0.5875(3) 0.1652(3) 0.2865(3) 0.029(3) Uani 0.522(5) 1 d PDU A 2 H3A_21 H 0.5455 0.1542 0.2600 0.034 Uiso 0.522(5) 1 calc PR A 2 H3B_21 H 0.5899 0.2016 0.2625 0.034 Uiso 0.522(5) 1 calc PR A 2 C4_21 C 0.6132(4) 0.1812(3) 0.3655(4) 0.042(4) Uani 0.522(5) 1 d PDU A 2 H4A_21 H 0.6536 0.1971 0.3905 0.051 Uiso 0.522(5) 1 calc PR A 2 H4B_21 H 0.5891 0.2137 0.3662 0.051 Uiso 0.522(5) 1 calc PR A 2 C5_21 C 0.6142(4) 0.1251(4) 0.4055(4) 0.038(4) Uani 0.522(5) 1 d PDU A 2 H5A_21 H 0.6339 0.1358 0.4573 0.045 Uiso 0.522(5) 1 calc PR A 2 H5B_21 H 0.5733 0.1128 0.3844 0.045 Uiso 0.522(5) 1 calc PR A 2 C6_21 C 0.6457(4) 0.0717(3) 0.4013(4) 0.037(4) Uani 0.522(5) 1 d PDU A 2 H6A_21 H 0.6424 0.0354 0.4247 0.044 Uiso 0.522(5) 1 calc PR A 2 H6B_21 H 0.6880 0.0817 0.4281 0.044 Uiso 0.522(5) 1 calc PR A 2 C7_21 C 0.6197(4) 0.0566(2) 0.3222(4) 0.030(3) Uani 0.522(5) 1 d PDU A 2 H7A_21 H 0.6427 0.0230 0.3210 0.036 Uiso 0.522(5) 1 calc PR A 2 H7B_21 H 0.5787 0.0421 0.2970 0.036 Uiso 0.522(5) 1 calc PR A 2 C1_3 C 0.5301(2) 0.2395(2) 0.0710(3) 0.0227(14) Uani 1 1 d U A . H1A_3 H 0.4905 0.2301 0.0261 0.027 Uiso 1 1 calc R . . H1B_3 H 0.5376 0.2096 0.1083 0.027 Uiso 1 1 calc R . . C2_3 C 0.52587(17) 0.30332(18) 0.0972(2) 0.0228(14) Uani 1 1 d DU . . H2_3 H 0.5430 0.3340 0.0822 0.027 Uiso 1 1 calc R A . C3_3 C 0.56144(17) 0.3057(2) 0.1797(2) 0.0418(18) Uani 1 1 d DU A . H3A_3 H 0.6030 0.2956 0.2017 0.050 Uiso 1 1 calc R . . H3B_3 H 0.5462 0.2745 0.1961 0.050 Uiso 1 1 calc R . . C4_3 C 0.55835(17) 0.3691(2) 0.20616(19) 0.056(2) Uani 1 1 d DU . . H4A_3 H 0.5794 0.3681 0.2596 0.068 Uiso 1 1 calc R A . H4B_3 H 0.5780 0.3996 0.1952 0.068 Uiso 1 1 calc R . . C5_3 C 0.4949(2) 0.3879(2) 0.1693(2) 0.058(2) Uani 1 1 d DU A . H5A_3 H 0.4772 0.3605 0.1859 0.070 Uiso 1 1 calc R . . H5B_3 H 0.4940 0.4303 0.1843 0.070 Uiso 1 1 calc R . . C6_3 C 0.45872(17) 0.38528(19) 0.0876(2) 0.0366(16) Uani 1 1 d DU . . H6A_3 H 0.4730 0.4166 0.0701 0.044 Uiso 1 1 calc R A . H6B_3 H 0.4172 0.3947 0.0663 0.044 Uiso 1 1 calc R . . C7_3 C 0.46254(15) 0.32189(19) 0.06226(19) 0.0280(15) Uani 1 1 d DU A . H7A_3 H 0.4441 0.2913 0.0749 0.034 Uiso 1 1 calc R . . H7B_3 H 0.4404 0.3221 0.0086 0.034 Uiso 1 1 calc R . . C1_4 C 0.5503(2) 0.2598(2) -0.0382(3) 0.0207(13) Uani 1 1 d U A . H1A_4 H 0.5829 0.2690 -0.0415 0.025 Uiso 1 1 calc R . . H1B_4 H 0.5249 0.2291 -0.0765 0.025 Uiso 1 1 calc R . . C2_4 C 0.51347(17) 0.31958(14) -0.0585(2) 0.0199(13) Uani 1 1 d DU . . H2_4 H 0.4908 0.3154 -0.0380 0.024 Uiso 1 1 calc R A . C3_4 C 0.55035(13) 0.37748(17) -0.02556(19) 0.0279(14) Uani 1 1 d DU A . H3A_4 H 0.5738 0.3832 -0.0443 0.034 Uiso 1 1 calc R . . H3B_4 H 0.5780 0.3728 0.0280 0.034 Uiso 1 1 calc R . . C4_4 C 0.51198(19) 0.43424(15) -0.0438(2) 0.0319(16) Uani 1 1 d DU . . H4A_4 H 0.4922 0.4309 -0.0200 0.038 Uiso 1 1 calc R A . H4B_4 H 0.5371 0.4714 -0.0248 0.038 Uiso 1 1 calc R . . C5_4 C 0.4662(2) 0.44020(15) -0.1255(2) 0.0427(18) Uani 1 1 d DU A . H5A_4 H 0.4400 0.4752 -0.1357 0.051 Uiso 1 1 calc R . . H5B_4 H 0.4862 0.4492 -0.1483 0.051 Uiso 1 1 calc R . . C6_4 C 0.42957(15) 0.3832(2) -0.1594(2) 0.0449(18) Uani 1 1 d DU . . H6A_4 H 0.4026 0.3882 -0.2130 0.054 Uiso 1 1 calc R A . H6B_4 H 0.4054 0.3770 -0.1417 0.054 Uiso 1 1 calc R . . C7_4 C 0.46856(19) 0.32712(16) -0.14041(19) 0.0360(16) Uani 1 1 d DU A . H7A_4 H 0.4436 0.2899 -0.1608 0.043 Uiso 1 1 calc R . . H7B_4 H 0.4893 0.3313 -0.1630 0.043 Uiso 1 1 calc R . . C1_5 C 0.6842(2) 0.1842(2) 0.0056(3) 0.0231(14) Uani 1 1 d U A . H1A_5 H 0.6843 0.2274 0.0190 0.028 Uiso 1 1 calc R . . H1B_5 H 0.7235 0.1765 0.0171 0.028 Uiso 1 1 calc R . . C2_5 C 0.63943(19) 0.18053(18) -0.07839(17) 0.0260(14) Uani 1 1 d DU . . H2_5 H 0.5991 0.1827 -0.0908 0.031 Uiso 1 1 calc R A . C3_5 C 0.64711(19) 0.23625(15) -0.1120(2) 0.0293(15) Uani 1 1 d DU A . H3A_5 H 0.6873 0.2361 -0.0990 0.035 Uiso 1 1 calc R . . H3B_5 H 0.6426 0.2740 -0.0917 0.035 Uiso 1 1 calc R . . C4_5 C 0.6022(2) 0.23686(16) -0.1951(2) 0.0430(18) Uani 1 1 d DU . . H4A_5 H 0.5622 0.2423 -0.2083 0.052 Uiso 1 1 calc R A . H4B_5 H 0.6105 0.2718 -0.2154 0.052 Uiso 1 1 calc R . . C5_5 C 0.6048(2) 0.1774(2) -0.22754(18) 0.0424(18) Uani 1 1 d DU A . H5A_5 H 0.5733 0.1776 -0.2807 0.051 Uiso 1 1 calc R . . H5B_5 H 0.6430 0.1751 -0.2201 0.051 Uiso 1 1 calc R . . C6_5 C 0.5979(2) 0.12167(17) -0.1945(2) 0.0436(17) Uani 1 1 d DU . . H6A_5 H 0.6031 0.0842 -0.2146 0.052 Uiso 1 1 calc R A . H6B_5 H 0.5577 0.1209 -0.2074 0.052 Uiso 1 1 calc R . . C7_5 C 0.64298(19) 0.12200(15) -0.1118(2) 0.0312(15) Uani 1 1 d DU A . H7A_5 H 0.6360 0.0862 -0.0911 0.037 Uiso 1 1 calc R . . H7B_5 H 0.6830 0.1181 -0.0990 0.037 Uiso 1 1 calc R . . C1_6 C 0.7154(9) 0.0703(9) 0.0654(10) 0.008(5) Uani 0.437(8) 1 d PU A 1 H1A_6 H 0.7104 0.0398 0.0935 0.010 Uiso 0.437(8) 1 calc PR A 1 H1B_6 H 0.6871 0.0574 0.0140 0.010 Uiso 0.437(8) 1 calc PR A 1 C2_6 C 0.7718(3) 0.0514(4) 0.0813(5) 0.014(4) Uani 0.437(8) 1 d PDU A 1 H2_6 H 0.7660 0.0612 0.0346 0.017 Uiso 0.437(8) 1 calc PR A 1 C3_6 C 0.8245(4) 0.0911(3) 0.1359(5) 0.024(4) Uani 0.437(8) 1 d PDU A 1 H3A_6 H 0.8375 0.0811 0.1857 0.029 Uiso 0.437(8) 1 calc PR A 1 H3B_6 H 0.8127 0.1348 0.1265 0.029 Uiso 0.437(8) 1 calc PR A 1 C4_6 C 0.8757(4) 0.0812(4) 0.1313(7) 0.025(5) Uani 0.437(8) 1 d PDU A 1 H4A_6 H 0.8645 0.0960 0.0836 0.030 Uiso 0.437(8) 1 calc PR A 1 H4B_6 H 0.9102 0.1053 0.1700 0.030 Uiso 0.437(8) 1 calc PR A 1 C5_6 C 0.8920(3) 0.0138(5) 0.1402(7) 0.039(8) Uani 0.437(8) 1 d PDU A 1 H5A_6 H 0.9230 0.0082 0.1331 0.046 Uiso 0.437(8) 1 calc PR A 1 H5B_6 H 0.9084 0.0009 0.1904 0.046 Uiso 0.437(8) 1 calc PR A 1 C6_6 C 0.8405(4) -0.0264(4) 0.0872(6) 0.037(4) Uani 0.437(8) 1 d PDU A 1 H6A_6 H 0.8526 -0.0700 0.0978 0.044 Uiso 0.437(8) 1 calc PR A 1 H6B_6 H 0.8272 -0.0174 0.0371 0.044 Uiso 0.437(8) 1 calc PR A 1 C7_6 C 0.7898(4) -0.0158(3) 0.0923(6) 0.018(4) Uani 0.437(8) 1 d PDU A 1 H7A_6 H 0.7556 -0.0409 0.0549 0.021 Uiso 0.437(8) 1 calc PR A 1 H7B_6 H 0.8017 -0.0293 0.1408 0.021 Uiso 0.437(8) 1 calc PR A 1 C1_61 C 0.7184(7) 0.0586(7) 0.0819(9) 0.020(4) Uani 0.563(8) 1 d PU A 2 H1A_61 H 0.7114 0.0313 0.1107 0.024 Uiso 0.563(8) 1 calc PR A 2 H1B_61 H 0.6987 0.0396 0.0333 0.024 Uiso 0.563(8) 1 calc PR A 2 C2_61 C 0.7832(3) 0.0592(4) 0.1178(5) 0.024(3) Uani 0.563(8) 1 d PDU A 2 H2_61 H 0.8023 0.0664 0.1707 0.029 Uiso 0.563(8) 1 calc PR A 2 C3_61 C 0.8136(3) 0.1026(3) 0.0980(4) 0.025(3) Uani 0.563(8) 1 d PDU A 2 H3A_61 H 0.8057 0.1455 0.1040 0.030 Uiso 0.563(8) 1 calc PR A 2 H3B_61 H 0.7972 0.0966 0.0461 0.030 Uiso 0.563(8) 1 calc PR A 2 C4_61 C 0.8801(3) 0.0918(4) 0.1455(6) 0.036(5) Uani 0.563(8) 1 d PDU A 2 H4A_61 H 0.8981 0.1185 0.1287 0.043 Uiso 0.563(8) 1 calc PR A 2 H4B_61 H 0.8974 0.1026 0.1966 0.043 Uiso 0.563(8) 1 calc PR A 2 C5_61 C 0.8936(3) 0.0252(5) 0.1415(6) 0.048(7) Uani 0.563(8) 1 d PDU A 2 H5A_61 H 0.8811 0.0162 0.0917 0.058 Uiso 0.563(8) 1 calc PR A 2 H5B_61 H 0.9366 0.0187 0.1756 0.058 Uiso 0.563(8) 1 calc PR A 2 C6_61 C 0.8634(4) -0.0186(3) 0.1602(5) 0.051(4) Uani 0.563(8) 1 d PDU A 2 H6A_61 H 0.8797 -0.0137 0.2121 0.061 Uiso 0.563(8) 1 calc PR A 2 H6B_61 H 0.8710 -0.0613 0.1530 0.061 Uiso 0.563(8) 1 calc PR A 2 C7_61 C 0.7973(3) -0.0070(3) 0.1126(6) 0.035(4) Uani 0.563(8) 1 d PDU A 2 H7A_61 H 0.7804 -0.0166 0.0613 0.041 Uiso 0.563(8) 1 calc PR A 2 H7B_61 H 0.7788 -0.0347 0.1280 0.041 Uiso 0.563(8) 1 calc PR A 2 C52 C 0.5256(2) 0.0208(2) 0.0297(3) 0.0179(13) Uani 1 1 d U . . H52 H 0.5382 0.0074 0.0789 0.021 Uiso 1 1 calc R . . C53 C 0.5076(2) 0.0888(2) 0.0182(3) 0.0168(13) Uani 1 1 d U . . H53 H 0.5013 0.1091 0.0497 0.020 Uiso 1 1 calc R A . C54 C 0.5009(2) 0.1194(2) -0.0391(3) 0.0200(13) Uani 1 1 d U A . H54 H 0.4753 0.1537 -0.0604 0.024 Uiso 1 1 calc R . . C55 C 0.5322(2) 0.0998(2) -0.0663(3) 0.0208(14) Uani 1 1 d U . . H55 H 0.5261 0.1186 -0.1078 0.025 Uiso 1 1 calc R A . C56 C 0.5727(2) 0.0514(2) -0.0294(3) 0.0195(13) Uani 1 1 d U A . H56 H 0.5963 0.0390 -0.0441 0.023 Uiso 1 1 calc R . . C57 C 0.5784(2) 0.0215(2) 0.0282(3) 0.0191(13) Uani 1 1 d U . . H57 H 0.6143 0.0021 0.0654 0.023 Uiso 1 1 calc R A . O1A O 0.7500 0.2500 0.5000 0.071(2) Uani 1 2 d SU . . C1A C 0.7435(6) 0.2649(7) 0.4321(8) 0.055(4) Uani 0.50 1 d PU B -1 H1A1 H 0.7568 0.3069 0.4323 0.066 Uiso 0.50 1 calc PR B -1 H1A2 H 0.7031 0.2581 0.3876 0.066 Uiso 0.50 1 calc PR B -1 C1B C 0.7972(6) 0.1992(6) 0.5129(7) 0.044(4) Uani 0.50 1 d PU B 2 H1A3 H 0.8374 0.2079 0.5569 0.053 Uiso 0.50 1 calc PR B 2 H1A4 H 0.7856 0.1570 0.5155 0.053 Uiso 0.50 1 calc PR B 2 C2A C 0.7916(3) 0.2098(3) 0.4454(4) 0.077(3) Uani 1 1 d U . . H2A1 H 0.7971 0.2127 0.4070 0.115 Uiso 1 1 calc R B -1 H2A2 H 0.7759 0.1692 0.4437 0.115 Uiso 1 1 calc R B -1 H2A3 H 0.8294 0.2158 0.4930 0.115 Uiso 1 1 calc R B -1 H2A4 H 0.8286 0.1991 0.4533 0.115 Uiso 1 1 calc R B 2 H2A5 H 0.7826 0.2531 0.4316 0.115 Uiso 1 1 calc R B 2 H2A6 H 0.7598 0.1842 0.4063 0.115 Uiso 1 1 calc R B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0131(4) 0.0172(4) 0.0150(4) -0.0003(4) 0.0067(4) -0.0003(4) P1 0.0174(8) 0.0166(8) 0.0153(8) 0.0011(7) 0.0067(7) 0.0050(7) P2 0.0135(8) 0.0206(8) 0.0143(8) -0.0017(7) 0.0061(7) -0.0020(7) P3 0.0150(8) 0.0204(9) 0.0184(8) -0.0050(7) 0.0090(7) -0.0032(7) B1 0.016(3) 0.019(3) 0.019(3) -0.001(3) 0.008(3) -0.003(3) C1 0.018(3) 0.018(3) 0.022(3) -0.002(2) 0.012(3) -0.005(2) C2 0.022(3) 0.023(3) 0.031(3) -0.006(3) 0.016(3) -0.003(3) C3 0.014(3) 0.040(4) 0.028(3) -0.009(3) 0.008(3) -0.004(3) C4 0.030(4) 0.025(3) 0.022(3) -0.003(3) 0.009(3) -0.006(3) C5 0.032(4) 0.028(4) 0.046(4) -0.015(3) 0.018(3) 0.000(3) C6 0.020(3) 0.034(4) 0.031(4) -0.009(3) 0.005(3) 0.005(3) C7 0.018(3) 0.020(3) 0.016(3) 0.000(2) 0.008(2) 0.006(2) C8 0.020(3) 0.019(3) 0.024(3) -0.001(2) 0.014(3) -0.001(2) C9 0.019(3) 0.014(3) 0.018(3) -0.003(2) 0.011(3) -0.004(2) C1_1 0.042(4) 0.029(4) 0.026(4) -0.003(3) 0.008(3) 0.017(3) C2_1 0.026(3) 0.016(3) 0.020(3) 0.002(2) 0.013(3) 0.006(3) C3_1 0.029(4) 0.038(4) 0.030(4) 0.013(3) 0.019(3) 0.006(3) C4_1 0.022(3) 0.051(4) 0.038(4) 0.011(3) 0.012(3) 0.004(3) C5_1 0.045(4) 0.049(4) 0.034(4) 0.019(3) 0.018(3) 0.018(3) C6_1 0.041(4) 0.034(4) 0.049(4) 0.023(3) 0.025(4) 0.010(3) C7_1 0.032(4) 0.036(4) 0.045(4) 0.006(3) 0.019(3) -0.001(3) C1_2 0.004(5) 0.005(5) 0.006(5) 0.000(2) 0.003(3) -0.001(2) C2_2 0.013(6) 0.015(6) 0.016(6) 0.011(5) 0.007(5) 0.008(5) C3_2 0.016(5) 0.012(6) 0.019(6) 0.005(4) 0.007(5) 0.006(4) C4_2 0.024(6) 0.036(7) 0.034(7) 0.002(5) 0.021(5) 0.008(5) C5_2 0.034(7) 0.022(6) 0.020(6) 0.001(5) 0.021(5) -0.003(5) C6_2 0.023(6) 0.039(7) 0.016(6) -0.007(5) 0.009(5) -0.005(6) C7_2 0.026(6) 0.025(7) 0.028(7) 0.006(5) 0.016(5) -0.002(5) C1_21 0.032(11) 0.028(8) 0.040(9) 0.001(6) 0.018(8) 0.003(7) C2_21 0.016(5) 0.020(6) 0.022(6) 0.000(5) 0.013(5) -0.001(5) C3_21 0.033(6) 0.025(6) 0.032(6) 0.007(5) 0.021(5) 0.005(5) C4_21 0.037(6) 0.049(7) 0.038(7) -0.010(5) 0.020(5) -0.010(5) C5_21 0.038(7) 0.041(7) 0.031(6) -0.009(5) 0.019(5) -0.007(6) C6_21 0.034(7) 0.048(7) 0.019(6) 0.012(5) 0.011(5) 0.001(6) C7_21 0.030(6) 0.019(6) 0.035(6) 0.007(5) 0.017(5) -0.002(5) C1_3 0.024(3) 0.020(3) 0.020(3) 0.010(3) 0.011(3) 0.004(3) C2_3 0.025(3) 0.031(3) 0.016(3) 0.008(3) 0.014(3) 0.012(3) C3_3 0.036(4) 0.066(5) 0.025(4) 0.006(3) 0.019(3) 0.021(3) C4_3 0.048(4) 0.081(5) 0.032(4) -0.009(4) 0.020(3) 0.031(4) C5_3 0.063(5) 0.081(5) 0.038(4) -0.003(4) 0.034(4) 0.026(4) C6_3 0.037(4) 0.047(4) 0.030(4) -0.003(3) 0.022(3) 0.010(3) C7_3 0.027(3) 0.033(3) 0.028(3) 0.000(3) 0.018(3) 0.007(3) C1_4 0.025(3) 0.018(3) 0.021(3) 0.000(2) 0.015(3) 0.002(2) C2_4 0.025(3) 0.018(3) 0.015(3) 0.000(2) 0.011(3) -0.002(3) C3_4 0.036(3) 0.019(3) 0.035(3) 0.001(3) 0.025(3) -0.005(3) C4_4 0.040(4) 0.020(3) 0.038(4) -0.010(3) 0.024(3) -0.005(3) C5_4 0.057(4) 0.023(4) 0.047(4) 0.011(3) 0.031(4) 0.005(3) C6_4 0.055(4) 0.026(4) 0.028(4) 0.001(3) 0.011(3) 0.009(3) C7_4 0.047(4) 0.029(3) 0.020(3) 0.002(3) 0.014(3) -0.001(3) C1_5 0.022(3) 0.030(3) 0.018(3) -0.004(3) 0.012(3) -0.004(3) C2_5 0.022(3) 0.041(4) 0.018(3) -0.006(3) 0.014(3) -0.012(3) C3_5 0.027(3) 0.036(4) 0.022(3) -0.008(3) 0.013(3) -0.010(3) C4_5 0.047(4) 0.041(4) 0.027(4) -0.002(3) 0.014(3) -0.002(3) C5_5 0.051(4) 0.042(4) 0.025(4) 0.001(3) 0.018(3) -0.007(3) C6_5 0.045(4) 0.055(4) 0.030(4) -0.018(3) 0.022(3) -0.017(4) C7_5 0.037(4) 0.035(4) 0.025(3) -0.009(3) 0.020(3) -0.012(3) C1_6 0.009(5) 0.008(5) 0.007(5) 0.001(3) 0.004(3) -0.002(3) C2_6 0.007(6) 0.013(6) 0.019(7) -0.001(5) 0.006(5) -0.002(5) C3_6 0.023(7) 0.016(7) 0.024(7) 0.004(6) 0.008(6) 0.000(5) C4_6 0.022(8) 0.019(8) 0.024(8) 0.001(6) 0.009(6) 0.007(6) C5_6 0.029(10) 0.043(9) 0.046(11) 0.006(7) 0.024(8) 0.017(7) C6_6 0.037(7) 0.045(8) 0.030(7) -0.004(6) 0.020(6) 0.010(6) C7_6 0.018(7) 0.014(7) 0.026(7) 0.002(5) 0.015(6) 0.010(5) C1_61 0.026(6) 0.023(7) 0.019(7) 0.006(5) 0.018(6) 0.001(5) C2_61 0.023(6) 0.019(6) 0.024(6) -0.014(5) 0.011(5) 0.004(5) C3_61 0.022(6) 0.026(6) 0.027(6) 0.000(5) 0.014(5) 0.006(4) C4_61 0.026(7) 0.037(7) 0.044(8) 0.010(6) 0.020(6) 0.007(5) C5_61 0.036(9) 0.057(9) 0.051(10) 0.003(6) 0.025(7) 0.003(6) C6_61 0.041(7) 0.045(7) 0.055(7) 0.018(6) 0.022(6) 0.011(5) C7_61 0.029(7) 0.025(7) 0.042(7) -0.002(5) 0.017(5) 0.005(5) C52 0.017(3) 0.019(3) 0.017(3) 0.003(2) 0.009(3) -0.001(2) C53 0.011(3) 0.019(3) 0.014(3) -0.003(2) 0.003(2) -0.004(2) C54 0.012(3) 0.017(3) 0.021(3) 0.003(3) 0.005(2) 0.001(2) C55 0.020(3) 0.027(3) 0.013(3) 0.006(2) 0.008(3) -0.005(3) C56 0.018(3) 0.016(3) 0.023(3) -0.010(3) 0.012(3) -0.005(2) C57 0.009(3) 0.023(3) 0.019(3) 0.000(3) 0.005(3) -0.002(2) O1A 0.087(5) 0.072(5) 0.071(5) -0.018(4) 0.057(4) -0.027(4) C1A 0.058(8) 0.064(8) 0.056(8) -0.001(6) 0.042(6) 0.001(6) C1B 0.049(7) 0.046(7) 0.048(7) -0.002(6) 0.035(6) -0.005(6) C2A 0.074(5) 0.083(6) 0.060(5) -0.012(4) 0.032(4) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C54 2.100(5) . yes Fe1 C56 2.103(5) . yes Fe1 C55 2.112(5) . yes Fe1 C53 2.174(5) . yes Fe1 C57 2.188(5) . yes Fe1 P2 2.2345(16) . yes Fe1 P3 2.2501(16) . yes Fe1 P1 2.2619(16) . yes P1 C1_21 1.78(3) . ? P1 C7 1.818(5) . ? P1 C1_1 1.844(6) . ? P1 C1_2 1.95(2) . ? P2 C8 1.810(5) . ? P2 C1_3 1.848(5) . ? P2 C1_4 1.859(5) . ? P3 C1_6 1.78(2) . ? P3 C9 1.833(5) . ? P3 C1_5 1.857(5) . ? P3 C1_61 1.937(17) . ? B1 C9 1.646(8) . ? B1 C1 1.650(8) . ? B1 C7 1.662(8) . ? B1 C8 1.661(8) . ? C1 C2 1.389(7) . ? C1 C6 1.400(7) . ? C2 C3 1.376(7) . ? C3 C4 1.403(7) . ? C4 C5 1.362(7) . ? C5 C6 1.367(7) . ? C1_1 C2_1 1.552(6) . ? C2_1 C7_1 1.520(3) . ? C2_1 C3_1 1.521(3) . ? C3_1 C4_1 1.531(3) . ? C4_1 C5_1 1.517(3) . ? C5_1 C6_1 1.503(3) . ? C6_1 C7_1 1.526(3) . ? C1_2 C2_2 1.52(2) . ? C2_2 C7_2 1.520(3) . ? C2_2 C3_2 1.520(3) . ? C3_2 C4_2 1.531(3) . ? C4_2 C5_2 1.516(3) . ? C5_2 C6_2 1.503(3) . ? C6_2 C7_2 1.526(3) . ? C1_21 C2_21 1.60(3) . ? C2_21 C7_21 1.520(3) . ? C2_21 C3_21 1.521(3) . ? C3_21 C4_21 1.531(3) . ? C4_21 C5_21 1.516(3) . ? C5_21 C6_21 1.503(3) . ? C6_21 C7_21 1.526(3) . ? C1_3 C2_3 1.546(6) . ? C2_3 C7_3 1.520(3) . ? C2_3 C3_3 1.521(3) . ? C3_3 C4_3 1.531(3) . ? C4_3 C5_3 1.516(3) . ? C5_3 C6_3 1.503(3) . ? C6_3 C7_3 1.526(3) . ? C1_4 C2_4 1.556(6) . ? C2_4 C7_4 1.520(3) . ? C2_4 C3_4 1.520(3) . ? C3_4 C4_4 1.531(3) . ? C4_4 C5_4 1.516(3) . ? C5_4 C6_4 1.503(3) . ? C6_4 C7_4 1.526(3) . ? C1_5 C2_5 1.548(6) . ? C2_5 C7_5 1.520(3) . ? C2_5 C3_5 1.520(3) . ? C3_5 C4_5 1.531(3) . ? C4_5 C5_5 1.516(3) . ? C5_5 C6_5 1.503(3) . ? C6_5 C7_5 1.526(3) . ? C1_6 C2_6 1.47(2) . ? C2_6 C7_6 1.520(3) . ? C2_6 C3_6 1.521(3) . ? C3_6 C4_6 1.531(3) . ? C4_6 C5_6 1.516(3) . ? C5_6 C6_6 1.503(3) . ? C6_6 C7_6 1.526(3) . ? C1_61 C2_61 1.497(18) . ? C2_61 C7_61 1.520(3) . ? C2_61 C3_61 1.521(3) . ? C3_61 C4_61 1.531(3) . ? C4_61 C5_61 1.516(3) . ? C5_61 C6_61 1.503(3) . ? C6_61 C7_61 1.526(3) . ? C52 C57 1.516(7) . ? C52 C53 1.538(7) . ? C52 C52 1.556(10) 5_655 ? C53 C54 1.379(7) . ? C54 C55 1.417(7) . ? C55 C56 1.410(7) . ? C56 C57 1.389(7) . ? O1A C1A 1.485(13) . ? O1A C1A 1.485(13) 7_656 ? O1A C1B 1.622(13) . ? O1A C1B 1.622(13) 7_656 ? C1A C2A 1.701(14) . ? C1B C2A 1.471(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C54 Fe1 C56 70.2(2) . . ? C54 Fe1 C55 39.32(19) . . ? C56 Fe1 C55 39.07(19) . . ? C54 Fe1 C53 37.59(18) . . ? C56 Fe1 C53 80.4(2) . . ? C55 Fe1 C53 68.84(19) . . ? C54 Fe1 C57 80.7(2) . . ? C56 Fe1 C57 37.70(18) . . ? C55 Fe1 C57 68.9(2) . . ? C53 Fe1 C57 66.26(19) . . ? C54 Fe1 P2 87.25(15) . . ? C56 Fe1 P2 140.41(16) . . ? C55 Fe1 P2 104.17(15) . . ? C53 Fe1 P2 101.44(14) . . ? C57 Fe1 P2 167.23(14) . . ? C54 Fe1 P3 142.44(15) . . ? C56 Fe1 P3 90.27(15) . . ? C55 Fe1 P3 106.64(15) . . ? C53 Fe1 P3 169.59(15) . . ? C57 Fe1 P3 103.47(14) . . ? P2 Fe1 P3 88.70(6) . . yes C54 Fe1 P1 127.66(15) . . ? C56 Fe1 P1 128.27(16) . . ? C55 Fe1 P1 157.46(15) . . ? C53 Fe1 P1 92.33(14) . . ? C57 Fe1 P1 92.59(15) . . ? P2 Fe1 P1 91.31(6) . . yes P3 Fe1 P1 89.74(6) . . yes C1_21 P1 C7 103.2(9) . . ? C1_21 P1 C1_1 97.2(8) . . ? C7 P1 C1_1 108.0(3) . . ? C1_21 P1 C1_2 7.2(12) . . ? C7 P1 C1_2 104.9(7) . . ? C1_1 P1 C1_2 103.1(7) . . ? C1_21 P1 Fe1 121.1(7) . . ? C7 P1 Fe1 113.86(17) . . ? C1_1 P1 Fe1 111.6(2) . . ? C1_2 P1 Fe1 114.5(6) . . ? C8 P2 C1_3 107.0(2) . . ? C8 P2 C1_4 106.5(2) . . ? C1_3 P2 C1_4 103.4(2) . . ? C8 P2 Fe1 116.53(18) . . ? C1_3 P2 Fe1 110.21(17) . . ? C1_4 P2 Fe1 112.22(17) . . ? C1_6 P3 C9 108.5(7) . . ? C1_6 P3 C1_5 96.5(6) . . ? C9 P3 C1_5 99.1(2) . . ? C1_6 P3 C1_61 12.1(8) . . ? C9 P3 C1_61 103.6(5) . . ? C1_5 P3 C1_61 108.4(5) . . ? C1_6 P3 Fe1 116.6(6) . . ? C9 P3 Fe1 114.56(17) . . ? C1_5 P3 Fe1 118.97(18) . . ? C1_61 P3 Fe1 110.7(5) . . ? C9 B1 C1 110.4(4) . . ? C9 B1 C7 109.0(4) . . ? C1 B1 C7 106.3(4) . . ? C9 B1 C8 110.1(4) . . ? C1 B1 C8 111.4(4) . . ? C7 B1 C8 109.5(4) . . ? C2 C1 C6 114.4(5) . . ? C2 C1 B1 122.0(5) . . ? C6 C1 B1 123.4(5) . . ? C3 C2 C1 123.0(5) . . ? C2 C3 C4 120.6(5) . . ? C5 C4 C3 117.1(5) . . ? C4 C5 C6 121.6(6) . . ? C5 C6 C1 123.2(6) . . ? B1 C7 P1 116.9(4) . . ? B1 C8 P2 115.6(4) . . ? B1 C9 P3 116.1(3) . . ? C2_1 C1_1 P1 121.3(4) . . ? C7_1 C2_1 C3_1 110.15(17) . . ? C7_1 C2_1 C1_1 109.7(3) . . ? C3_1 C2_1 C1_1 112.5(4) . . ? C2_1 C3_1 C4_1 111.63(18) . . ? C5_1 C4_1 C3_1 110.56(19) . . ? C6_1 C5_1 C4_1 112.65(18) . . ? C5_1 C6_1 C7_1 110.87(18) . . ? C2_1 C7_1 C6_1 111.77(18) . . ? C2_2 C1_2 P1 124.2(12) . . ? C7_2 C2_2 C3_2 110.16(18) . . ? C7_2 C2_2 C1_2 111.2(10) . . ? C3_2 C2_2 C1_2 107.5(9) . . ? C2_2 C3_2 C4_2 111.70(18) . . ? C5_2 C4_2 C3_2 110.62(19) . . ? C6_2 C5_2 C4_2 112.67(19) . . ? C5_2 C6_2 C7_2 110.84(19) . . ? C2_2 C7_2 C6_2 111.73(19) . . ? C2_21 C1_21 P1 120.1(14) . . ? C7_21 C2_21 C3_21 110.14(18) . . ? C7_21 C2_21 C1_21 110.9(11) . . ? C3_21 C2_21 C1_21 112.6(10) . . ? C2_21 C3_21 C4_21 111.68(18) . . ? C5_21 C4_21 C3_21 110.64(19) . . ? C6_21 C5_21 C4_21 112.69(19) . . ? C5_21 C6_21 C7_21 110.84(19) . . ? C2_21 C7_21 C6_21 111.70(19) . . ? C2_3 C1_3 P2 122.8(3) . . ? C7_3 C2_3 C3_3 110.12(17) . . ? C7_3 C2_3 C1_3 112.0(3) . . ? C3_3 C2_3 C1_3 111.3(3) . . ? C2_3 C3_3 C4_3 111.68(18) . . ? C5_3 C4_3 C3_3 110.62(19) . . ? C6_3 C5_3 C4_3 112.68(19) . . ? C5_3 C6_3 C7_3 110.83(18) . . ? C2_3 C7_3 C6_3 111.71(18) . . ? C2_4 C1_4 P2 120.4(3) . . ? C7_4 C2_4 C3_4 110.13(17) . . ? C7_4 C2_4 C1_4 112.2(3) . . ? C3_4 C2_4 C1_4 114.0(3) . . ? C2_4 C3_4 C4_4 111.66(18) . . ? C5_4 C4_4 C3_4 110.61(19) . . ? C6_4 C5_4 C4_4 112.67(18) . . ? C5_4 C6_4 C7_4 110.83(18) . . ? C2_4 C7_4 C6_4 111.69(18) . . ? C2_5 C1_5 P3 123.5(3) . . ? C7_5 C2_5 C3_5 110.14(17) . . ? C7_5 C2_5 C1_5 114.5(3) . . ? C3_5 C2_5 C1_5 109.0(3) . . ? C2_5 C3_5 C4_5 111.72(18) . . ? C5_5 C4_5 C3_5 110.66(19) . . ? C6_5 C5_5 C4_5 112.70(19) . . ? C5_5 C6_5 C7_5 110.82(18) . . ? C2_5 C7_5 C6_5 111.67(18) . . ? C2_6 C1_6 P3 140.8(13) . . ? C1_6 C2_6 C7_6 121.1(9) . . ? C1_6 C2_6 C3_6 115.6(10) . . ? C7_6 C2_6 C3_6 110.14(18) . . ? C2_6 C3_6 C4_6 111.68(18) . . ? C5_6 C4_6 C3_6 110.63(19) . . ? C6_6 C5_6 C4_6 112.69(19) . . ? C5_6 C6_6 C7_6 110.85(19) . . ? C2_6 C7_6 C6_6 111.72(19) . . ? C2_61 C1_61 P3 118.2(10) . . ? C1_61 C2_61 C7_61 104.1(8) . . ? C1_61 C2_61 C3_61 124.6(8) . . ? C7_61 C2_61 C3_61 110.14(18) . . ? C2_61 C3_61 C4_61 111.66(18) . . ? C5_61 C4_61 C3_61 110.60(19) . . ? C6_61 C5_61 C4_61 112.67(19) . . ? C5_61 C6_61 C7_61 110.85(19) . . ? C2_61 C7_61 C6_61 111.72(19) . . ? C57 C52 C53 102.6(4) . . ? C57 C52 C52 113.9(5) . 5_655 ? C53 C52 C52 111.7(5) . 5_655 ? C54 C53 C52 118.2(5) . . ? C54 C53 Fe1 68.3(3) . . ? C52 C53 Fe1 93.7(3) . . ? C53 C54 C55 120.2(5) . . ? C53 C54 Fe1 74.1(3) . . ? C55 C54 Fe1 70.8(3) . . ? C56 C55 C54 117.5(5) . . ? C56 C55 Fe1 70.1(3) . . ? C54 C55 Fe1 69.9(3) . . ? C57 C56 C55 120.9(5) . . ? C57 C56 Fe1 74.5(3) . . ? C55 C56 Fe1 70.8(3) . . ? C56 C57 C52 117.7(5) . . ? C56 C57 Fe1 67.9(3) . . ? C52 C57 Fe1 93.7(3) . . ? C1A O1A C1A 180.0(12) . 7_656 ? C1A O1A C1B 85.1(7) . . ? C1A O1A C1B 94.9(7) 7_656 . ? C1A O1A C1B 94.9(7) . 7_656 ? C1A O1A C1B 85.1(7) 7_656 7_656 ? C1B O1A C1B 179.997(4) . 7_656 ? O1A C1A C2A 94.1(8) . . ? C2A C1B O1A 98.0(8) . . ? C1B C2A C1A 82.7(7) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.619 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 604498' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C114 H188 B2 Fe2 N2 P6, 2(C4 H8 O), 2(C H2 Cl2)' _chemical_formula_sum 'C124 H208 B2 Cl4 Fe2 N2 O2 P6' _chemical_formula_weight 2219.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.7338(16) _cell_length_b 15.5757(11) _cell_length_c 17.6503(13) _cell_angle_alpha 90.00 _cell_angle_beta 110.2880(10) _cell_angle_gamma 90.00 _cell_volume 5862.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8425 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.56 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2404 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8338 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 3 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38965 _diffrn_reflns_av_R_equivalents 0.0902 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.95 _reflns_number_total 9196 _reflns_number_gt 5139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule was highly disordered, and the disorder was modelled with the use of free variables and appropriate restraints. All disorders were refined with the help of similarity restraints on 1-2 and 1-3 distances and displacement parameters as well as rigid bond restraints for anisotropic displacement parameters. All close contacts, both inter and intramolecular, reported by the Platon validation software involve at least one partner from a minor component of a disorder. While it is conceivable that more solvent molecules and parts of the compounds are disordered and parameterization of these disordered components would remove the close contacts, the data at hand did not allow for further modeling of the disorder. The dataset is 99.6 % complete to theta = 23.01. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9196 _refine_ls_number_parameters 764 _refine_ls_number_restraints 5918 _refine_ls_R_factor_all 0.1743 _refine_ls_R_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 2.946 _refine_ls_restrained_S_all 2.452 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.32832(4) 0.99572(6) 1.00932(5) 0.0383(3) Uani 1 1 d U . . P1 P 0.32321(7) 1.03031(10) 0.88345(10) 0.0356(5) Uani 1 1 d U . . P2 P 0.24560(7) 1.07943(11) 0.99523(10) 0.0359(5) Uani 1 1 d U A . P3 P 0.26192(8) 0.88644(11) 0.95846(11) 0.0389(5) Uani 1 1 d U B . N1 N 0.4909(3) 1.0362(3) 1.0133(3) 0.0578(17) Uani 1 1 d U . . B1 B 0.1868(3) 1.0050(5) 0.8345(4) 0.0333(18) Uani 1 1 d U . . C1 C 0.1222(3) 1.0086(4) 0.7568(4) 0.0319(15) Uani 1 1 d U . . C2 C 0.0682(3) 0.9637(4) 0.7562(4) 0.0500(19) Uani 1 1 d U . . H2 H 0.0704 0.9314 0.8027 0.060 Uiso 1 1 calc R . . C3 C 0.0121(3) 0.9639(4) 0.6918(4) 0.052(2) Uani 1 1 d U . . H3 H -0.0227 0.9316 0.6940 0.062 Uiso 1 1 calc R . . C4 C 0.0076(3) 1.0118(4) 0.6245(4) 0.0438(17) Uani 1 1 d U . . H4 H -0.0308 1.0129 0.5800 0.053 Uiso 1 1 calc R . . C5 C 0.0574(3) 1.0572(4) 0.6210(4) 0.0374(17) Uani 1 1 d U . . H5 H 0.0540 1.0906 0.5746 0.045 Uiso 1 1 calc R . . C6 C 0.1140(3) 1.0546(4) 0.6864(4) 0.0359(16) Uani 1 1 d U . . H6 H 0.1487 1.0859 0.6824 0.043 Uiso 1 1 calc R . . C7 C 0.2456(2) 1.0496(4) 0.8123(3) 0.0356(16) Uani 1 1 d U . . H7A H 0.2386 1.1124 0.8076 0.043 Uiso 1 1 calc R . . H7B H 0.2439 1.0282 0.7588 0.043 Uiso 1 1 calc R . . C8 C 0.1755(2) 1.0569(4) 0.9087(3) 0.0344(16) Uani 1 1 d U . . H8A H 0.1463 1.0230 0.9275 0.041 Uiso 1 1 calc R . . H8B H 0.1546 1.1120 0.8875 0.041 Uiso 1 1 calc R . . C9 C 0.2041(3) 0.9046(4) 0.8599(3) 0.0417(17) Uani 1 1 d U . . H9A H 0.2192 0.8778 0.8192 0.050 Uiso 1 1 calc R . . H9B H 0.1650 0.8746 0.8573 0.050 Uiso 1 1 calc R . . C1_1 C 0.3575(3) 0.9430(4) 0.8430(4) 0.0425(18) Uani 1 1 d U . . H1A_1 H 0.4000 0.9322 0.8823 0.051 Uiso 1 1 calc R . . H1B_1 H 0.3323 0.8908 0.8419 0.051 Uiso 1 1 calc R . . C2_1 C 0.3635(3) 0.9519(4) 0.7593(3) 0.067(2) Uani 1 1 d DU . . H2_1 H 0.3528 1.0122 0.7400 0.081 Uiso 1 1 calc R . . C3_1 C 0.3183(2) 0.8910(5) 0.6986(4) 0.119(3) Uani 1 1 d DU . . H3A_1 H 0.3273 0.8312 0.7183 0.143 Uiso 1 1 calc R . . H3B_1 H 0.2747 0.9047 0.6941 0.143 Uiso 1 1 calc R . . C4_1 C 0.3244(3) 0.8982(6) 0.6159(3) 0.228(6) Uani 1 1 d DU . . H4A_1 H 0.3117 0.9563 0.5935 0.274 Uiso 1 1 calc R . . H4B_1 H 0.2966 0.8558 0.5786 0.274 Uiso 1 1 calc R . . C5_1 C 0.3934(4) 0.8811(6) 0.6237(4) 0.191(5) Uani 1 1 d DU . . H5A_1 H 0.4040 0.8206 0.6398 0.229 Uiso 1 1 calc R . . H5B_1 H 0.3979 0.8896 0.5703 0.229 Uiso 1 1 calc R . . C6_1 C 0.4383(3) 0.9383(6) 0.6837(5) 0.224(6) Uani 1 1 d DU . . H6A_1 H 0.4316 0.9983 0.6640 0.269 Uiso 1 1 calc R . . H6B_1 H 0.4817 0.9217 0.6898 0.269 Uiso 1 1 calc R . . C7_1 C 0.4300(2) 0.9330(5) 0.7641(4) 0.151(4) Uani 1 1 d DU . . H7A_1 H 0.4587 0.9744 0.8016 0.181 Uiso 1 1 calc R . . H7B_1 H 0.4417 0.8747 0.7866 0.181 Uiso 1 1 calc R . . C1_2 C 0.3711(3) 1.1220(4) 0.8772(4) 0.057(2) Uani 1 1 d U . . H1A_2 H 0.3701 1.1619 0.9204 0.068 Uiso 1 1 calc R . . H1B_2 H 0.4146 1.1002 0.8935 0.068 Uiso 1 1 calc R . . C2_2 C 0.3621(3) 1.1755(3) 0.8057(4) 0.135(4) Uani 1 1 d DU . . H2_2 H 0.3424 1.1369 0.7584 0.163 Uiso 1 1 calc R . . C3_2 C 0.4268(3) 1.1976(4) 0.8025(5) 0.158(4) Uani 1 1 d DU . . H3A_2 H 0.4536 1.1457 0.8154 0.190 Uiso 1 1 calc R . . H3B_2 H 0.4224 1.2162 0.7472 0.190 Uiso 1 1 calc R . . C4_2 C 0.4581(2) 1.2685(5) 0.8618(5) 0.198(5) Uani 1 1 d DU . . H4A_2 H 0.4987 1.2838 0.8564 0.238 Uiso 1 1 calc R . . H4B_2 H 0.4662 1.2485 0.9177 0.238 Uiso 1 1 calc R . . C5_2 C 0.4146(3) 1.3481(3) 0.8441(5) 0.157(4) Uani 1 1 d DU . . H5A_2 H 0.4338 1.3929 0.8850 0.188 Uiso 1 1 calc R . . H5B_2 H 0.4108 1.3717 0.7905 0.188 Uiso 1 1 calc R . . C6_2 C 0.3509(3) 1.3278(4) 0.8450(4) 0.132(4) Uani 1 1 d DU . . H6A_2 H 0.3240 1.3794 0.8288 0.158 Uiso 1 1 calc R . . H6B_2 H 0.3539 1.3121 0.9005 0.158 Uiso 1 1 calc R . . C7_2 C 0.3217(2) 1.2554(5) 0.7887(4) 0.107(3) Uani 1 1 d DU . . H7A_2 H 0.3140 1.2742 0.7325 0.128 Uiso 1 1 calc R . . H7B_2 H 0.2807 1.2413 0.7935 0.128 Uiso 1 1 calc R . . C1_3 C 0.2631(3) 1.1925(4) 0.9805(4) 0.0455(18) Uani 1 1 d U . . H1A_3 H 0.3037 1.2057 1.0233 0.055 Uiso 0.692(6) 1 calc PR A 1 H1B_3 H 0.2707 1.1948 0.9286 0.055 Uiso 0.692(6) 1 calc PR A 1 H1C_3 H 0.3076 1.2033 1.0130 0.055 Uiso 0.308(6) 1 calc PR A 2 H1D_3 H 0.2585 1.2002 0.9230 0.055 Uiso 0.308(6) 1 calc PR A 2 C2_3 C 0.2191(3) 1.2680(3) 0.9793(4) 0.043(3) Uani 0.692(6) 1 d PDU A 1 H2_3 H 0.1797 1.2436 0.9835 0.052 Uiso 0.692(6) 1 calc PR A 1 C3_3 C 0.2014(4) 1.3180(5) 0.8998(3) 0.070(4) Uani 0.692(6) 1 d PDU A 1 H3A_3 H 0.2398 1.3423 0.8939 0.083 Uiso 0.692(6) 1 calc PR A 1 H3B_3 H 0.1822 1.2783 0.8541 0.083 Uiso 0.692(6) 1 calc PR A 1 C4_3 C 0.1557(3) 1.3900(5) 0.8970(4) 0.093(4) Uani 0.692(6) 1 d PDU A 1 H4A_3 H 0.1157 1.3657 0.8977 0.111 Uiso 0.692(6) 1 calc PR A 1 H4B_3 H 0.1470 1.4233 0.8465 0.111 Uiso 0.692(6) 1 calc PR A 1 C5_3 C 0.1845(4) 1.4494(3) 0.9710(5) 0.075(4) Uani 0.692(6) 1 d PDU A 1 H5A_3 H 0.2217 1.4787 0.9662 0.090 Uiso 0.692(6) 1 calc PR A 1 H5B_3 H 0.1535 1.4940 0.9709 0.090 Uiso 0.692(6) 1 calc PR A 1 C6_3 C 0.2033(4) 1.4020(5) 1.0488(4) 0.066(3) Uani 0.692(6) 1 d PDU A 1 H6A_3 H 0.1655 1.3794 1.0574 0.079 Uiso 0.692(6) 1 calc PR A 1 H6B_3 H 0.2246 1.4418 1.0936 0.079 Uiso 0.692(6) 1 calc PR A 1 C7_3 C 0.2465(3) 1.3291(4) 1.0494(3) 0.051(3) Uani 0.692(6) 1 d PDU A 1 H7A_3 H 0.2560 1.2969 1.1006 0.061 Uiso 0.692(6) 1 calc PR A 1 H7B_3 H 0.2864 1.3526 1.0475 0.061 Uiso 0.692(6) 1 calc PR A 1 C1_4 C 0.2235(3) 1.0850(4) 1.0865(3) 0.0424(17) Uani 1 1 d U . . H1A_4 H 0.2353 1.0287 1.1135 0.051 Uiso 0.591(17) 1 calc PR A 1 H1B_4 H 0.2523 1.1275 1.1223 0.051 Uiso 0.591(17) 1 calc PR A 1 H1C_4 H 0.2233 1.0259 1.1071 0.051 Uiso 0.409(17) 1 calc PR A 2 H1D_4 H 0.2564 1.1174 1.1285 0.051 Uiso 0.409(17) 1 calc PR A 2 C2_4 C 0.1595(3) 1.1052(6) 1.0905(6) 0.024(3) Uani 0.591(17) 1 d PDU A 1 H2_4 H 0.1367 1.1390 1.0408 0.028 Uiso 0.591(17) 1 calc PR A 1 C3_4 C 0.1182(3) 1.0276(6) 1.0905(7) 0.036(3) Uani 0.591(17) 1 d PDU A 1 H3A_4 H 0.1140 0.9913 1.0428 0.043 Uiso 0.591(17) 1 calc PR A 1 H3B_4 H 0.1385 0.9929 1.1395 0.043 Uiso 0.591(17) 1 calc PR A 1 C4_4 C 0.0536(3) 1.0551(7) 1.0882(6) 0.047(4) Uani 0.591(17) 1 d PDU A 1 H4A_4 H 0.0287 1.0039 1.0916 0.056 Uiso 0.591(17) 1 calc PR A 1 H4B_4 H 0.0313 1.0850 1.0368 0.056 Uiso 0.591(17) 1 calc PR A 1 C5_4 C 0.0604(4) 1.1158(8) 1.1603(6) 0.050(4) Uani 0.591(17) 1 d PDU A 1 H5A_4 H 0.0183 1.1367 1.1565 0.061 Uiso 0.591(17) 1 calc PR A 1 H5B_4 H 0.0780 1.0831 1.2113 0.061 Uiso 0.591(17) 1 calc PR A 1 C6_4 C 0.1014(4) 1.1906(6) 1.1625(8) 0.042(4) Uani 0.591(17) 1 d PDU A 1 H6A_4 H 0.1071 1.2246 1.2119 0.051 Uiso 0.591(17) 1 calc PR A 1 H6B_4 H 0.0811 1.2279 1.1152 0.051 Uiso 0.591(17) 1 calc PR A 1 C7_4 C 0.1642(3) 1.1625(6) 1.1616(7) 0.038(4) Uani 0.591(17) 1 d PDU A 1 H7A_4 H 0.1865 1.1313 1.2123 0.046 Uiso 0.591(17) 1 calc PR A 1 H7B_4 H 0.1893 1.2139 1.1599 0.046 Uiso 0.591(17) 1 calc PR A 1 C1_5 C 0.2198(3) 0.8616(4) 1.0274(4) 0.0450(18) Uani 1 1 d U . . H1A_5 H 0.2511 0.8629 1.0828 0.054 Uiso 0.764(6) 1 calc PR B 1 H1B_5 H 0.1905 0.9097 1.0237 0.054 Uiso 0.764(6) 1 calc PR B 1 H1C_5 H 0.2523 0.8507 1.0808 0.054 Uiso 0.236(6) 1 calc PR B 2 H1D_5 H 0.1983 0.9152 1.0330 0.054 Uiso 0.236(6) 1 calc PR B 2 C2_5 C 0.1805(2) 0.7751(4) 1.0200(3) 0.040(3) Uani 0.764(6) 1 d PDU B 1 H2_5 H 0.2043 0.7268 1.0069 0.048 Uiso 0.764(6) 1 calc PR B 1 C3_5 C 0.1750(3) 0.7583(4) 1.1027(3) 0.048(3) Uani 0.764(6) 1 d PDU B 1 H3A_5 H 0.2175 0.7539 1.1439 0.057 Uiso 0.764(6) 1 calc PR B 1 H3B_5 H 0.1532 0.8072 1.1173 0.057 Uiso 0.764(6) 1 calc PR B 1 C4_5 C 0.1390(3) 0.6762(4) 1.1026(3) 0.055(3) Uani 0.764(6) 1 d PDU B 1 H4A_5 H 0.1339 0.6687 1.1557 0.066 Uiso 0.764(6) 1 calc PR B 1 H4B_5 H 0.1626 0.6263 1.0932 0.066 Uiso 0.764(6) 1 calc PR B 1 C5_5 C 0.0738(3) 0.6812(4) 1.0351(4) 0.053(3) Uani 0.764(6) 1 d PDU B 1 H5A_5 H 0.0516 0.6260 1.0328 0.063 Uiso 0.764(6) 1 calc PR B 1 H5B_5 H 0.0488 0.7269 1.0486 0.063 Uiso 0.764(6) 1 calc PR B 1 C6_5 C 0.0780(3) 0.6993(4) 0.9545(3) 0.045(3) Uani 0.764(6) 1 d PDU B 1 H6A_5 H 0.0353 0.7066 0.9145 0.054 Uiso 0.764(6) 1 calc PR B 1 H6B_5 H 0.0978 0.6499 0.9373 0.054 Uiso 0.764(6) 1 calc PR B 1 C7_5 C 0.1156(3) 0.7787(4) 0.9563(3) 0.050(3) Uani 0.764(6) 1 d PDU B 1 H7A_5 H 0.0929 0.8289 0.9669 0.059 Uiso 0.764(6) 1 calc PR B 1 H7B_5 H 0.1196 0.7869 0.9027 0.059 Uiso 0.764(6) 1 calc PR B 1 C1_6 C 0.3032(3) 0.7836(4) 0.9563(4) 0.058(2) Uani 1 1 d U . . H1A_6 H 0.3478 0.7978 0.9675 0.069 Uiso 0.639(4) 1 calc PR B 1 H1B_6 H 0.3015 0.7487 1.0024 0.069 Uiso 0.639(4) 1 calc PR B 1 H1C_6 H 0.3417 0.7982 0.9449 0.069 Uiso 0.361(4) 1 calc PR B 2 H1D_6 H 0.3169 0.7596 1.0117 0.069 Uiso 0.361(4) 1 calc PR B 2 C2_6 C 0.2821(3) 0.7240(3) 0.8802(5) 0.055(3) Uani 0.639(4) 1 d PDU B 1 H2_6 H 0.2723 0.7607 0.8308 0.066 Uiso 0.639(4) 1 calc PR B 1 C3_6 C 0.2237(3) 0.6717(5) 0.8742(4) 0.051(3) Uani 0.639(4) 1 d PDU B 1 H3A_6 H 0.2322 0.6370 0.9239 0.062 Uiso 0.639(4) 1 calc PR B 1 H3B_6 H 0.1887 0.7113 0.8703 0.062 Uiso 0.639(4) 1 calc PR B 1 C4_6 C 0.2045(3) 0.6128(5) 0.8013(5) 0.077(4) Uani 0.639(4) 1 d PDU B 1 H4A_6 H 0.1919 0.6474 0.7511 0.092 Uiso 0.639(4) 1 calc PR B 1 H4B_6 H 0.1683 0.5773 0.8007 0.092 Uiso 0.639(4) 1 calc PR B 1 C5_6 C 0.2605(4) 0.5541(4) 0.8051(5) 0.099(5) Uani 0.639(4) 1 d PDU B 1 H5A_6 H 0.2694 0.5149 0.8519 0.119 Uiso 0.639(4) 1 calc PR B 1 H5B_6 H 0.2488 0.5186 0.7556 0.119 Uiso 0.639(4) 1 calc PR B 1 C6_6 C 0.3182(3) 0.6035(5) 0.8127(5) 0.094(4) Uani 0.639(4) 1 d PDU B 1 H6A_6 H 0.3114 0.6367 0.7625 0.112 Uiso 0.639(4) 1 calc PR B 1 H6B_6 H 0.3533 0.5632 0.8195 0.112 Uiso 0.639(4) 1 calc PR B 1 C7_6 C 0.3350(2) 0.6637(5) 0.8832(5) 0.062(3) Uani 0.639(4) 1 d PDU B 1 H7A_6 H 0.3720 0.6979 0.8844 0.074 Uiso 0.639(4) 1 calc PR B 1 H7B_6 H 0.3468 0.6298 0.9337 0.074 Uiso 0.639(4) 1 calc PR B 1 C2_31 C 0.2240(4) 1.2601(6) 1.0018(9) 0.043(7) Uiso 0.308(6) 1 d PDU A 2 H2_31 H 0.2193 1.2418 1.0537 0.051 Uiso 0.308(6) 1 calc PR A 2 C3_31 C 0.1578(5) 1.2772(6) 0.9423(8) 0.041(6) Uiso 0.308(6) 1 d PDU A 2 H3A_31 H 0.1603 1.2965 0.8900 0.049 Uiso 0.308(6) 1 calc PR A 2 H3B_31 H 0.1333 1.2233 0.9326 0.049 Uiso 0.308(6) 1 calc PR A 2 C4_31 C 0.1244(3) 1.3451(7) 0.9741(9) 0.058(7) Uiso 0.308(6) 1 d PDU A 2 H4A_31 H 0.1181 1.3240 1.0236 0.070 Uiso 0.308(6) 1 calc PR A 2 H4B_31 H 0.0828 1.3574 0.9331 0.070 Uiso 0.308(6) 1 calc PR A 2 C5_31 C 0.1645(5) 1.4280(6) 0.9932(10) 0.064(7) Uiso 0.308(6) 1 d PDU A 2 H5A_31 H 0.1663 1.4524 0.9423 0.077 Uiso 0.308(6) 1 calc PR A 2 H5B_31 H 0.1440 1.4708 1.0174 0.077 Uiso 0.308(6) 1 calc PR A 2 C6_31 C 0.2294(5) 1.4126(8) 1.0496(9) 0.069(7) Uiso 0.308(6) 1 d PDU A 2 H6A_31 H 0.2282 1.3960 1.1032 0.082 Uiso 0.308(6) 1 calc PR A 2 H6B_31 H 0.2540 1.4663 1.0563 0.082 Uiso 0.308(6) 1 calc PR A 2 C7_31 C 0.2609(3) 1.3432(8) 1.0189(10) 0.046(7) Uiso 0.308(6) 1 d PDU A 2 H7A_31 H 0.3029 1.3322 1.0594 0.055 Uiso 0.308(6) 1 calc PR A 2 H7B_31 H 0.2667 1.3631 0.9687 0.055 Uiso 0.308(6) 1 calc PR A 2 C2_41 C 0.1557(4) 1.1292(8) 1.0754(9) 0.024(5) Uiso 0.409(17) 1 d PDU A 2 H2_41 H 0.1419 1.1680 1.0273 0.029 Uiso 0.409(17) 1 calc PR A 2 C3_41 C 0.1090(4) 1.0557(7) 1.0660(8) 0.028(5) Uiso 0.409(17) 1 d PDU A 2 H3A_41 H 0.1031 1.0249 1.0148 0.033 Uiso 0.409(17) 1 calc PR A 2 H3B_41 H 0.1263 1.0145 1.1110 0.033 Uiso 0.409(17) 1 calc PR A 2 C4_41 C 0.0461(4) 1.0884(9) 1.0658(8) 0.046(6) Uiso 0.409(17) 1 d PDU A 2 H4A_41 H 0.0177 1.0394 1.0629 0.055 Uiso 0.409(17) 1 calc PR A 2 H4B_41 H 0.0266 1.1253 1.0179 0.055 Uiso 0.409(17) 1 calc PR A 2 C5_41 C 0.0559(5) 1.1405(10) 1.1439(9) 0.041(5) Uiso 0.409(17) 1 d PDU A 2 H5A_41 H 0.0152 1.1650 1.1419 0.049 Uiso 0.409(17) 1 calc PR A 2 H5B_41 H 0.0705 1.1014 1.1910 0.049 Uiso 0.409(17) 1 calc PR A 2 C6_41 C 0.1020(6) 1.2112(9) 1.1552(10) 0.041(6) Uiso 0.409(17) 1 d PDU A 2 H6A_41 H 0.1092 1.2393 1.2079 0.049 Uiso 0.409(17) 1 calc PR A 2 H6B_41 H 0.0848 1.2547 1.1123 0.049 Uiso 0.409(17) 1 calc PR A 2 C7_41 C 0.1631(4) 1.1783(9) 1.1522(10) 0.037(6) Uiso 0.409(17) 1 d PDU A 2 H7A_41 H 0.1826 1.1403 1.1991 0.045 Uiso 0.409(17) 1 calc PR A 2 H7B_41 H 0.1917 1.2274 1.1565 0.045 Uiso 0.409(17) 1 calc PR A 2 C2_51 C 0.1725(5) 0.7914(8) 1.0149(11) 0.032(7) Uiso 0.236(6) 1 d PDU B 2 H2_51 H 0.1660 0.7647 0.9610 0.039 Uiso 0.236(6) 1 calc PR B 2 C3_51 C 0.2019(4) 0.7235(8) 1.0797(11) 0.045(7) Uiso 0.236(6) 1 d PDU B 2 H3A_51 H 0.2428 0.7055 1.0768 0.054 Uiso 0.236(6) 1 calc PR B 2 H3B_51 H 0.2095 0.7488 1.1338 0.054 Uiso 0.236(6) 1 calc PR B 2 C4_51 C 0.1598(6) 0.6456(6) 1.0689(12) 0.037(7) Uiso 0.236(6) 1 d PDU B 2 H4A_51 H 0.1786 0.6043 1.1134 0.044 Uiso 0.236(6) 1 calc PR B 2 H4B_51 H 0.1552 0.6167 1.0172 0.044 Uiso 0.236(6) 1 calc PR B 2 C5_51 C 0.0946(6) 0.6744(9) 1.0691(12) 0.041(8) Uiso 0.236(6) 1 d PDU B 2 H5A_51 H 0.0664 0.6240 1.0584 0.049 Uiso 0.236(6) 1 calc PR B 2 H5B_51 H 0.0991 0.6968 1.1233 0.049 Uiso 0.236(6) 1 calc PR B 2 C6_51 C 0.0658(4) 0.7417(10) 1.0078(13) 0.057(8) Uiso 0.236(6) 1 d PDU B 2 H6A_51 H 0.0261 0.7613 1.0134 0.068 Uiso 0.236(6) 1 calc PR B 2 H6B_51 H 0.0558 0.7171 0.9530 0.068 Uiso 0.236(6) 1 calc PR B 2 C7_51 C 0.1089(6) 0.8167(8) 1.0173(12) 0.047(8) Uiso 0.236(6) 1 d PDU B 2 H7A_51 H 0.1146 0.8455 1.0694 0.056 Uiso 0.236(6) 1 calc PR B 2 H7B_51 H 0.0893 0.8586 0.9735 0.056 Uiso 0.236(6) 1 calc PR B 2 C2_61 C 0.2701(8) 0.7104(9) 0.8979(10) 0.069(7) Uiso 0.361(4) 1 d PDU B 2 H2_61 H 0.2235 0.7176 0.8794 0.083 Uiso 0.361(4) 1 calc PR B 2 C3_61 C 0.2895(9) 0.6254(12) 0.9431(7) 0.143(11) Uiso 0.361(4) 1 d PDU B 2 H3A_61 H 0.3359 0.6220 0.9657 0.172 Uiso 0.361(4) 1 calc PR B 2 H3B_61 H 0.2737 0.6234 0.9887 0.172 Uiso 0.361(4) 1 calc PR B 2 C4_61 C 0.2641(9) 0.5491(9) 0.8880(12) 0.131(9) Uiso 0.361(4) 1 d PDU B 2 H4A_61 H 0.2177 0.5491 0.8693 0.158 Uiso 0.361(4) 1 calc PR B 2 H4B_61 H 0.2794 0.4951 0.9178 0.158 Uiso 0.361(4) 1 calc PR B 2 C5_61 C 0.2862(9) 0.5549(9) 0.8144(11) 0.099(8) Uiso 0.361(4) 1 d PDU B 2 H5A_61 H 0.3324 0.5479 0.8332 0.119 Uiso 0.361(4) 1 calc PR B 2 H5B_61 H 0.2673 0.5072 0.7768 0.119 Uiso 0.361(4) 1 calc PR B 2 C6_61 C 0.2690(9) 0.6378(12) 0.7706(7) 0.123(8) Uiso 0.361(4) 1 d PDU B 2 H6A_61 H 0.2228 0.6414 0.7452 0.148 Uiso 0.361(4) 1 calc PR B 2 H6B_61 H 0.2872 0.6402 0.7271 0.148 Uiso 0.361(4) 1 calc PR B 2 C7_61 C 0.2924(8) 0.7124(9) 0.8264(11) 0.103(7) Uiso 0.361(4) 1 d PDU B 2 H7A_61 H 0.2779 0.7663 0.7959 0.124 Uiso 0.361(4) 1 calc PR B 2 H7B_61 H 0.3388 0.7125 0.8464 0.124 Uiso 0.361(4) 1 calc PR B 2 C52 C 0.4439(3) 1.0103(5) 1.0452(4) 0.054(2) Uani 1 1 d U . . C53 C 0.4129(3) 1.0776(5) 1.0677(4) 0.0497(19) Uani 1 1 d U . . H53 H 0.4163 1.1343 1.0499 0.060 Uiso 1 1 calc R . . C54 C 0.3771(3) 1.0621(4) 1.1158(4) 0.0483(19) Uani 1 1 d U . . H54 H 0.3615 1.1096 1.1368 0.058 Uiso 1 1 calc R . . C55 C 0.3633(3) 0.9787(5) 1.1345(4) 0.0474(19) Uani 1 1 d U . . H55 H 0.3410 0.9692 1.1704 0.057 Uiso 1 1 calc R . . C56 C 0.3832(3) 0.9103(5) 1.0987(4) 0.0505(19) Uani 1 1 d U . . H56 H 0.3731 0.8531 1.1082 0.061 Uiso 1 1 calc R . . C57 C 0.4188(3) 0.9264(5) 1.0478(4) 0.0502(19) Uani 1 1 d U . . H57 H 0.4260 0.8814 1.0156 0.060 Uiso 1 1 calc R . . C61_7 C 0.9942(8) 0.1806(15) 0.7661(10) 0.126(8) Uani 0.583(4) 1 d PDU C 1 H61A_7 H 0.9936 0.2301 0.7306 0.151 Uiso 0.583(4) 1 calc PR C 1 H61B_7 H 1.0166 0.1329 0.7508 0.151 Uiso 0.583(4) 1 calc PR C 1 Cl1_7 Cl 1.03403(18) 0.2090(4) 0.8657(3) 0.144(3) Uani 0.583(4) 1 d PDU C 1 Cl2_7 Cl 0.92099(19) 0.1505(4) 0.7517(3) 0.152(3) Uani 0.583(4) 1 d PDU C 1 C61_71 C 1.0049(11) 0.1530(9) 0.7834(12) 0.068(7) Uani 0.417(4) 1 d PDU C 2 H61A_71 H 0.9822 0.1182 0.7352 0.081 Uiso 0.417(4) 1 calc PR C 2 H61B_71 H 1.0498 0.1540 0.7890 0.081 Uiso 0.417(4) 1 calc PR C 2 Cl1_71 Cl 0.9758(3) 0.2569(3) 0.7695(4) 0.102(3) Uani 0.417(4) 1 d PDU C 2 Cl2_71 Cl 0.9975(3) 0.1077(3) 0.8647(3) 0.100(3) Uani 0.417(4) 1 d PDU C 2 C1_8 C 0.5105(8) 0.656(3) 0.7730(10) 0.497(19) Uiso 0.639(4) 1 d PDU B 2 H1A_8 H 0.5016 0.6956 0.7265 0.597 Uiso 0.639(4) 1 calc PR B 2 H1B_8 H 0.5180 0.5980 0.7552 0.597 Uiso 0.639(4) 1 calc PR B 2 C2_8 C 0.5683(5) 0.6863(12) 0.8418(12) 0.201(8) Uiso 0.639(4) 1 d PDU B 2 H2A_8 H 0.5832 0.7423 0.8289 0.242 Uiso 0.639(4) 1 calc PR B 2 H2B_8 H 0.6027 0.6439 0.8532 0.242 Uiso 0.639(4) 1 calc PR B 2 C3_8 C 0.5455(7) 0.6943(13) 0.9132(8) 0.203(9) Uiso 0.639(4) 1 d PDU B 2 H3A_8 H 0.5508 0.6396 0.9434 0.244 Uiso 0.639(4) 1 calc PR B 2 H3B_8 H 0.5683 0.7403 0.9506 0.244 Uiso 0.639(4) 1 calc PR B 2 C4_8 C 0.4770(7) 0.7166(12) 0.8734(11) 0.276(11) Uiso 0.639(4) 1 d PDU B 2 H4A_8 H 0.4715 0.7770 0.8547 0.332 Uiso 0.639(4) 1 calc PR B 2 H4B_8 H 0.4534 0.7070 0.9104 0.332 Uiso 0.639(4) 1 calc PR B 2 O_8 O 0.4561(4) 0.6537(6) 0.8015(6) 0.126(4) Uiso 0.639(4) 1 d PDU B 2 C1_81 C 0.5994(9) 0.6005(16) 0.9900(19) 0.305(18) Uiso 0.361(4) 1 d PDU B 1 H1A_81 H 0.6381 0.5763 0.9848 0.366 Uiso 0.361(4) 1 calc PR B 1 H1B_81 H 0.6086 0.6188 1.0466 0.366 Uiso 0.361(4) 1 calc PR B 1 C2_81 C 0.5481(12) 0.5352(9) 0.9665(16) 0.151(11) Uiso 0.361(4) 1 d PDU B 1 H2A_81 H 0.5433 0.5089 1.0151 0.181 Uiso 0.361(4) 1 calc PR B 1 H2B_81 H 0.5573 0.4893 0.9334 0.181 Uiso 0.361(4) 1 calc PR B 1 C3_81 C 0.4895(8) 0.5832(15) 0.9184(16) 0.163(12) Uiso 0.361(4) 1 d PDU B 1 H3A_81 H 0.4559 0.5737 0.9412 0.195 Uiso 0.361(4) 1 calc PR B 1 H3B_81 H 0.4744 0.5641 0.8613 0.195 Uiso 0.361(4) 1 calc PR B 1 C4_81 C 0.5082(8) 0.6765(13) 0.925(2) 0.202(13) Uiso 0.361(4) 1 d PDU B 1 H4A_81 H 0.4831 0.7082 0.8753 0.242 Uiso 0.361(4) 1 calc PR B 1 H4B_81 H 0.5022 0.7037 0.9720 0.242 Uiso 0.361(4) 1 calc PR B 1 O_81 O 0.5765(6) 0.6758(8) 0.9333(8) 0.064(4) Uiso 0.361(4) 1 d PDU B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0246(5) 0.0524(7) 0.0407(6) 0.0047(5) 0.0151(4) 0.0022(5) P1 0.0231(10) 0.0448(12) 0.0417(12) 0.0062(9) 0.0149(9) 0.0018(8) P2 0.0224(10) 0.0453(12) 0.0414(12) -0.0073(9) 0.0129(9) -0.0043(8) P3 0.0371(11) 0.0425(12) 0.0440(12) 0.0036(9) 0.0228(10) 0.0042(9) N1 0.052(4) 0.043(4) 0.053(4) 0.006(3) -0.013(3) 0.016(3) B1 0.027(4) 0.040(5) 0.036(4) -0.001(4) 0.014(3) -0.005(4) C1 0.027(3) 0.036(4) 0.037(4) -0.014(3) 0.017(3) -0.003(3) C2 0.045(4) 0.076(5) 0.035(4) -0.006(3) 0.021(4) -0.019(4) C3 0.038(4) 0.073(5) 0.046(5) -0.013(4) 0.016(4) -0.020(4) C4 0.027(4) 0.064(5) 0.037(4) -0.012(4) 0.007(3) -0.007(4) C5 0.031(4) 0.042(4) 0.036(4) 0.001(3) 0.008(3) 0.002(3) C6 0.025(4) 0.041(4) 0.042(4) -0.007(3) 0.011(3) -0.005(3) C7 0.024(3) 0.044(4) 0.043(4) 0.003(3) 0.017(3) 0.002(3) C8 0.022(3) 0.039(4) 0.043(4) -0.004(3) 0.013(3) 0.001(3) C9 0.034(4) 0.049(5) 0.048(4) -0.004(3) 0.022(3) -0.006(3) C1_1 0.031(4) 0.055(4) 0.051(4) -0.001(3) 0.025(3) 0.008(3) C2_1 0.082(5) 0.054(5) 0.081(6) -0.025(4) 0.046(5) -0.001(4) C3_1 0.084(6) 0.190(8) 0.088(6) -0.023(6) 0.037(5) 0.029(6) C4_1 0.189(10) 0.314(11) 0.190(10) -0.023(9) 0.078(8) 0.050(9) C5_1 0.142(9) 0.288(10) 0.160(9) -0.078(8) 0.076(7) 0.000(8) C6_1 0.193(9) 0.301(11) 0.214(10) -0.087(9) 0.116(8) -0.080(8) C7_1 0.099(7) 0.291(10) 0.084(7) -0.059(6) 0.058(6) -0.067(7) C1_2 0.045(4) 0.068(5) 0.057(5) 0.021(4) 0.017(4) -0.008(4) C2_2 0.087(7) 0.178(8) 0.144(8) 0.042(7) 0.044(6) -0.037(6) C3_2 0.154(8) 0.193(9) 0.167(8) 0.056(7) 0.105(7) 0.014(7) C4_2 0.102(8) 0.166(9) 0.267(10) -0.022(8) -0.013(7) -0.019(7) C5_2 0.121(8) 0.152(8) 0.197(9) 0.044(7) 0.055(7) -0.018(7) C6_2 0.089(7) 0.184(9) 0.135(8) 0.015(7) 0.053(6) -0.001(6) C7_2 0.081(6) 0.100(7) 0.133(7) 0.052(6) 0.029(6) 0.022(5) C1_3 0.034(4) 0.043(4) 0.055(5) -0.008(3) 0.011(3) -0.010(3) C2_3 0.033(6) 0.039(6) 0.055(6) -0.012(5) 0.011(5) -0.001(4) C3_3 0.069(7) 0.068(7) 0.057(7) -0.016(6) 0.004(6) 0.014(6) C4_3 0.077(8) 0.088(8) 0.096(8) 0.010(7) 0.007(6) 0.024(6) C5_3 0.068(7) 0.060(7) 0.101(8) 0.001(6) 0.035(6) 0.023(5) C6_3 0.074(7) 0.056(7) 0.077(7) -0.012(5) 0.036(6) 0.011(6) C7_3 0.064(6) 0.043(6) 0.055(6) 0.003(5) 0.032(5) 0.002(5) C1_4 0.041(4) 0.051(4) 0.043(4) -0.009(3) 0.025(3) -0.007(3) C2_4 0.021(6) 0.023(6) 0.027(6) 0.015(5) 0.008(4) 0.014(4) C3_4 0.032(6) 0.031(7) 0.046(7) 0.002(6) 0.016(5) 0.000(5) C4_4 0.033(6) 0.059(7) 0.049(7) 0.009(6) 0.015(5) -0.010(5) C5_4 0.043(7) 0.068(8) 0.050(7) 0.010(6) 0.029(5) 0.007(6) C6_4 0.029(6) 0.043(7) 0.060(7) -0.020(6) 0.020(5) -0.006(5) C7_4 0.024(6) 0.047(7) 0.041(7) 0.005(6) 0.008(5) -0.003(5) C1_5 0.045(4) 0.056(5) 0.043(4) 0.011(3) 0.027(4) -0.006(3) C2_5 0.042(5) 0.049(6) 0.037(5) -0.005(4) 0.023(4) -0.003(4) C3_5 0.049(5) 0.054(6) 0.043(5) 0.011(4) 0.019(4) -0.006(5) C4_5 0.065(6) 0.059(6) 0.044(6) 0.027(5) 0.023(5) -0.001(5) C5_5 0.045(5) 0.052(6) 0.063(6) -0.009(5) 0.021(5) -0.024(4) C6_5 0.043(5) 0.052(6) 0.039(5) 0.004(4) 0.013(4) -0.016(4) C7_5 0.065(6) 0.049(5) 0.038(5) 0.012(4) 0.022(5) -0.015(5) C1_6 0.064(5) 0.060(5) 0.063(5) 0.013(4) 0.039(4) 0.014(4) C2_6 0.074(7) 0.041(6) 0.059(7) 0.003(5) 0.034(6) 0.014(6) C3_6 0.071(7) 0.049(6) 0.043(6) -0.012(5) 0.031(6) -0.012(5) C4_6 0.111(8) 0.062(7) 0.063(7) -0.011(6) 0.037(7) -0.026(6) C5_6 0.149(9) 0.073(8) 0.080(8) -0.025(6) 0.046(7) -0.003(7) C6_6 0.126(9) 0.085(8) 0.078(7) -0.016(6) 0.047(7) 0.042(7) C7_6 0.082(7) 0.058(7) 0.056(7) -0.002(5) 0.036(6) 0.021(6) C52 0.032(4) 0.084(6) 0.043(4) 0.021(4) 0.009(3) -0.001(4) C53 0.025(4) 0.079(5) 0.047(5) 0.010(4) 0.015(4) -0.008(4) C54 0.038(4) 0.059(5) 0.041(4) 0.006(4) 0.005(4) -0.001(4) C55 0.032(4) 0.072(5) 0.036(4) 0.002(4) 0.009(3) -0.003(4) C56 0.035(4) 0.068(5) 0.044(4) 0.008(4) 0.008(4) 0.014(4) C57 0.029(4) 0.074(5) 0.044(4) 0.003(4) 0.008(4) 0.019(4) C61_7 0.122(12) 0.172(13) 0.120(12) -0.006(10) 0.089(10) 0.003(10) Cl1_7 0.089(3) 0.175(5) 0.149(5) -0.085(4) 0.016(3) 0.049(3) Cl2_7 0.082(4) 0.231(6) 0.148(5) -0.078(4) 0.048(3) 0.001(3) C61_71 0.054(10) 0.105(12) 0.057(11) -0.019(9) 0.035(9) 0.022(8) Cl1_71 0.143(6) 0.070(4) 0.139(5) 0.024(4) 0.108(5) 0.021(4) Cl2_71 0.117(5) 0.121(5) 0.083(4) 0.025(4) 0.060(4) 0.046(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C55 2.089(6) . yes Fe1 C54 2.094(6) . yes Fe1 C56 2.110(6) . yes Fe1 C57 2.212(6) . yes Fe1 P2 2.2303(18) . yes Fe1 C53 2.238(6) . yes Fe1 P3 2.245(2) . yes Fe1 P1 2.2496(18) . yes Fe1 C52 2.491(7) . yes P1 C7 1.801(5) . ? P1 C1_2 1.821(6) . ? P1 C1_1 1.830(5) . ? P2 C8 1.819(5) . ? P2 C1_3 1.843(6) . ? P2 C1_4 1.849(5) . ? P3 C9 1.802(6) . ? P3 C1_5 1.833(5) . ? P3 C1_6 1.863(6) . ? N1 N1 1.340(9) 3_677 yes N1 C52 1.429(8) . yes B1 C1 1.625(8) . ? B1 C8 1.634(8) . ? B1 C9 1.636(9) . ? B1 C7 1.668(8) . ? C1 C6 1.390(7) . ? C1 C2 1.411(7) . ? C2 C3 1.382(8) . ? C3 C4 1.376(8) . ? C4 C5 1.355(7) . ? C5 C6 1.401(7) . ? C1_1 C2_1 1.536(7) . ? C2_1 C7_1 1.514(4) . ? C2_1 C3_1 1.530(4) . ? C3_1 C4_1 1.518(4) . ? C4_1 C5_1 1.549(4) . ? C5_1 C6_1 1.486(4) . ? C6_1 C7_1 1.497(4) . ? C1_2 C2_2 1.467(8) . ? C2_2 C7_2 1.514(4) . ? C2_2 C3_2 1.530(4) . ? C3_2 C4_2 1.518(4) . ? C4_2 C5_2 1.549(4) . ? C5_2 C6_2 1.486(4) . ? C6_2 C7_2 1.497(4) . ? C1_3 C2_31 1.509(11) . ? C1_3 C2_3 1.540(7) . ? C2_3 C7_3 1.514(4) . ? C2_3 C3_3 1.530(4) . ? C3_3 C4_3 1.517(4) . ? C4_3 C5_3 1.549(4) . ? C5_3 C6_3 1.486(4) . ? C6_3 C7_3 1.498(4) . ? C1_4 C2_4 1.513(8) . ? C1_4 C2_41 1.637(11) . ? C2_4 C7_4 1.514(4) . ? C2_4 C3_4 1.530(4) . ? C3_4 C4_4 1.517(4) . ? C4_4 C5_4 1.549(4) . ? C5_4 C6_4 1.486(4) . ? C6_4 C7_4 1.498(4) . ? C1_5 C2_51 1.495(12) . ? C1_5 C2_5 1.595(7) . ? C2_5 C7_5 1.514(4) . ? C2_5 C3_5 1.530(4) . ? C3_5 C4_5 1.517(4) . ? C4_5 C5_5 1.549(4) . ? C5_5 C6_5 1.486(4) . ? C6_5 C7_5 1.498(4) . ? C1_6 C2_61 1.547(15) . ? C1_6 C2_6 1.566(9) . ? C2_6 C7_6 1.514(4) . ? C2_6 C3_6 1.530(4) . ? C3_6 C4_6 1.517(4) . ? C4_6 C5_6 1.548(4) . ? C5_6 C6_6 1.486(4) . ? C6_6 C7_6 1.498(4) . ? C2_31 C7_31 1.514(4) . ? C2_31 C3_31 1.530(4) . ? C3_31 C4_31 1.517(4) . ? C4_31 C5_31 1.549(4) . ? C5_31 C6_31 1.486(4) . ? C6_31 C7_31 1.497(4) . ? C2_41 C7_41 1.514(4) . ? C2_41 C3_41 1.530(4) . ? C3_41 C4_41 1.517(4) . ? C4_41 C5_41 1.549(4) . ? C5_41 C6_41 1.486(4) . ? C6_41 C7_41 1.497(4) . ? C2_51 C7_51 1.514(4) . ? C2_51 C3_51 1.530(4) . ? C3_51 C4_51 1.517(4) . ? C4_51 C5_51 1.549(4) . ? C5_51 C6_51 1.486(4) . ? C6_51 C7_51 1.497(4) . ? C2_61 C7_61 1.514(4) . ? C2_61 C3_61 1.530(4) . ? C3_61 C4_61 1.517(4) . ? C4_61 C5_61 1.549(4) . ? C5_61 C6_61 1.486(4) . ? C6_61 C7_61 1.497(4) . ? C52 C53 1.396(8) . ? C52 C57 1.433(9) . ? C53 C54 1.384(8) . ? C54 C55 1.403(8) . ? C55 C56 1.392(8) . ? C56 C57 1.425(8) . ? C61_7 Cl2_7 1.661(14) . ? C61_7 Cl1_7 1.734(16) . ? C61_71 Cl2_71 1.661(14) . ? C61_71 Cl1_71 1.734(16) . ? C1_8 O_8 1.489(8) . ? C1_8 C2_8 1.522(8) . ? C2_8 C3_8 1.525(8) . ? C3_8 C4_8 1.511(8) . ? C4_8 O_8 1.541(8) . ? C1_81 C2_81 1.494(8) . ? C1_81 O_81 1.511(8) . ? C2_81 C3_81 1.506(8) . ? C3_81 C4_81 1.508(8) . ? C4_81 O_81 1.506(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C55 Fe1 C54 39.2(2) . . ? C55 Fe1 C56 38.7(2) . . ? C54 Fe1 C56 69.4(3) . . ? C55 Fe1 C57 69.0(2) . . ? C54 Fe1 C57 79.5(3) . . ? C56 Fe1 C57 38.4(2) . . ? C55 Fe1 P2 100.89(19) . . ? C54 Fe1 P2 88.58(19) . . ? C56 Fe1 P2 135.2(2) . . ? C57 Fe1 P2 168.05(19) . . ? C55 Fe1 C53 68.6(2) . . ? C54 Fe1 C53 37.1(2) . . ? C56 Fe1 C53 79.9(3) . . ? C57 Fe1 C53 65.0(3) . . ? P2 Fe1 C53 106.0(2) . . ? C55 Fe1 P3 106.4(2) . . ? C54 Fe1 P3 143.8(2) . . ? C56 Fe1 P3 87.8(2) . . ? C57 Fe1 P3 100.2(2) . . ? P2 Fe1 P3 88.54(7) . . ? C53 Fe1 P3 165.2(2) . . ? C55 Fe1 P1 160.94(18) . . ? C54 Fe1 P1 126.7(2) . . ? C56 Fe1 P1 134.8(2) . . ? C57 Fe1 P1 98.31(18) . . ? P2 Fe1 P1 89.83(7) . . ? C53 Fe1 P1 93.46(17) . . ? P3 Fe1 P1 89.39(7) . . ? C55 Fe1 C52 76.2(2) . . ? C54 Fe1 C52 62.8(2) . . ? C56 Fe1 C52 64.5(2) . . ? C57 Fe1 C52 34.9(2) . . ? P2 Fe1 C52 138.6(2) . . ? C53 Fe1 C52 33.8(2) . . ? P3 Fe1 C52 132.4(2) . . ? P1 Fe1 C52 85.30(16) . . ? C7 P1 C1_2 106.8(3) . . ? C7 P1 C1_1 107.4(3) . . ? C1_2 P1 C1_1 102.4(3) . . ? C7 P1 Fe1 115.51(18) . . ? C1_2 P1 Fe1 114.9(2) . . ? C1_1 P1 Fe1 108.9(2) . . ? C8 P2 C1_3 103.6(3) . . ? C8 P2 C1_4 108.5(3) . . ? C1_3 P2 C1_4 102.4(3) . . ? C8 P2 Fe1 116.12(19) . . ? C1_3 P2 Fe1 111.0(2) . . ? C1_4 P2 Fe1 113.8(2) . . ? C9 P3 C1_5 107.4(3) . . ? C9 P3 C1_6 108.6(3) . . ? C1_5 P3 C1_6 102.4(3) . . ? C9 P3 Fe1 115.6(2) . . ? C1_5 P3 Fe1 109.2(2) . . ? C1_6 P3 Fe1 112.7(2) . . ? N1 N1 C52 105.3(7) 3_677 . ? C1 B1 C8 108.1(5) . . ? C1 B1 C9 109.0(5) . . ? C8 B1 C9 110.0(5) . . ? C1 B1 C7 110.5(5) . . ? C8 B1 C7 110.1(5) . . ? C9 B1 C7 109.1(5) . . ? C6 C1 C2 113.7(5) . . ? C6 C1 B1 125.0(5) . . ? C2 C1 B1 121.3(6) . . ? C3 C2 C1 123.9(6) . . ? C4 C3 C2 118.9(6) . . ? C5 C4 C3 120.6(6) . . ? C4 C5 C6 119.4(6) . . ? C1 C6 C5 123.5(6) . . ? B1 C7 P1 116.0(4) . . ? B1 C8 P2 115.6(4) . . ? B1 C9 P3 116.1(4) . . ? C2_1 C1_1 P1 120.0(4) . . ? C7_1 C2_1 C3_1 109.4(2) . . ? C7_1 C2_1 C1_1 110.4(5) . . ? C3_1 C2_1 C1_1 110.9(5) . . ? C4_1 C3_1 C2_1 111.4(3) . . ? C3_1 C4_1 C5_1 109.3(2) . . ? C6_1 C5_1 C4_1 112.5(3) . . ? C5_1 C6_1 C7_1 111.2(3) . . ? C6_1 C7_1 C2_1 112.8(2) . . ? C2_2 C1_2 P1 126.2(5) . . ? C1_2 C2_2 C7_2 122.1(5) . . ? C1_2 C2_2 C3_2 108.1(5) . . ? C7_2 C2_2 C3_2 109.5(2) . . ? C4_2 C3_2 C2_2 111.4(3) . . ? C3_2 C4_2 C5_2 109.2(2) . . ? C6_2 C5_2 C4_2 112.6(3) . . ? C5_2 C6_2 C7_2 111.3(3) . . ? C6_2 C7_2 C2_2 112.9(2) . . ? C2_31 C1_3 P2 117.2(6) . . ? C2_3 C1_3 P2 124.1(4) . . ? C7_3 C2_3 C3_3 109.5(2) . . ? C7_3 C2_3 C1_3 112.8(5) . . ? C3_3 C2_3 C1_3 111.4(5) . . ? C4_3 C3_3 C2_3 111.5(3) . . ? C3_3 C4_3 C5_3 109.3(2) . . ? C6_3 C5_3 C4_3 112.6(3) . . ? C5_3 C6_3 C7_3 111.2(3) . . ? C6_3 C7_3 C2_3 112.8(2) . . ? C2_4 C1_4 P2 127.4(5) . . ? C2_41 C1_4 P2 116.4(6) . . ? C7_4 C2_4 C1_4 111.7(6) . . ? C7_4 C2_4 C3_4 109.5(2) . . ? C1_4 C2_4 C3_4 115.8(6) . . ? C4_4 C3_4 C2_4 111.5(3) . . ? C3_4 C4_4 C5_4 109.3(2) . . ? C6_4 C5_4 C4_4 112.6(3) . . ? C5_4 C6_4 C7_4 111.2(3) . . ? C6_4 C7_4 C2_4 112.8(2) . . ? C2_51 C1_5 P3 124.8(8) . . ? C2_5 C1_5 P3 122.0(4) . . ? C7_5 C2_5 C3_5 109.5(2) . . ? C7_5 C2_5 C1_5 113.8(5) . . ? C3_5 C2_5 C1_5 107.1(4) . . ? C4_5 C3_5 C2_5 111.5(3) . . ? C3_5 C4_5 C5_5 109.3(2) . . ? C6_5 C5_5 C4_5 112.6(2) . . ? C5_5 C6_5 C7_5 111.2(3) . . ? C6_5 C7_5 C2_5 112.8(2) . . ? C2_61 C1_6 P3 121.0(7) . . ? C2_6 C1_6 P3 121.4(5) . . ? C7_6 C2_6 C3_6 109.5(2) . . ? C7_6 C2_6 C1_6 109.6(5) . . ? C3_6 C2_6 C1_6 112.0(5) . . ? C4_6 C3_6 C2_6 111.5(3) . . ? C3_6 C4_6 C5_6 109.3(2) . . ? C6_6 C5_6 C4_6 112.6(3) . . ? C5_6 C6_6 C7_6 111.2(3) . . ? C6_6 C7_6 C2_6 112.8(2) . . ? C1_3 C2_31 C7_31 108.2(7) . . ? C1_3 C2_31 C3_31 118.4(9) . . ? C7_31 C2_31 C3_31 109.5(2) . . ? C4_31 C3_31 C2_31 111.5(3) . . ? C3_31 C4_31 C5_31 109.3(2) . . ? C6_31 C5_31 C4_31 112.6(3) . . ? C5_31 C6_31 C7_31 111.2(3) . . ? C6_31 C7_31 C2_31 112.8(2) . . ? C7_41 C2_41 C3_41 109.5(2) . . ? C7_41 C2_41 C1_4 107.3(7) . . ? C3_41 C2_41 C1_4 106.6(7) . . ? C4_41 C3_41 C2_41 111.5(3) . . ? C3_41 C4_41 C5_41 109.3(2) . . ? C6_41 C5_41 C4_41 112.6(3) . . ? C5_41 C6_41 C7_41 111.2(3) . . ? C6_41 C7_41 C2_41 112.8(2) . . ? C1_5 C2_51 C7_51 116.7(9) . . ? C1_5 C2_51 C3_51 106.8(9) . . ? C7_51 C2_51 C3_51 109.5(2) . . ? C4_51 C3_51 C2_51 111.5(3) . . ? C3_51 C4_51 C5_51 109.3(2) . . ? C6_51 C5_51 C4_51 112.6(3) . . ? C5_51 C6_51 C7_51 111.2(3) . . ? C6_51 C7_51 C2_51 112.8(2) . . ? C7_61 C2_61 C3_61 109.5(2) . . ? C7_61 C2_61 C1_6 108.3(12) . . ? C3_61 C2_61 C1_6 107.7(12) . . ? C4_61 C3_61 C2_61 111.4(3) . . ? C3_61 C4_61 C5_61 109.3(2) . . ? C6_61 C5_61 C4_61 112.6(3) . . ? C5_61 C6_61 C7_61 111.2(3) . . ? C6_61 C7_61 C2_61 112.8(2) . . ? C53 C52 N1 114.9(7) . . ? C53 C52 C57 115.4(6) . . ? N1 C52 C57 129.1(7) . . ? C53 C52 Fe1 63.1(4) . . ? N1 C52 Fe1 142.5(4) . . ? C57 C52 Fe1 61.9(3) . . ? C54 C53 C52 120.4(7) . . ? C54 C53 Fe1 65.8(4) . . ? C52 C53 Fe1 83.1(4) . . ? C53 C54 C55 122.2(7) . . ? C53 C54 Fe1 77.1(4) . . ? C55 C54 Fe1 70.2(4) . . ? C56 C55 C54 117.9(6) . . ? C56 C55 Fe1 71.5(4) . . ? C54 C55 Fe1 70.6(4) . . ? C55 C56 C57 119.8(7) . . ? C55 C56 Fe1 69.8(4) . . ? C57 C56 Fe1 74.7(4) . . ? C56 C57 C52 120.0(6) . . ? C56 C57 Fe1 66.9(3) . . ? C52 C57 Fe1 83.3(4) . . ? Cl2_7 C61_7 Cl1_7 111.7(6) . . ? Cl2_71 C61_71 Cl1_71 111.7(6) . . ? O_8 C1_8 C2_8 109.0(6) . . ? C1_8 C2_8 C3_8 103.8(5) . . ? C4_8 C3_8 C2_8 103.0(7) . . ? C3_8 C4_8 O_8 102.2(6) . . ? C1_8 O_8 C4_8 102.0(10) . . ? C2_81 C1_81 O_81 106.7(7) . . ? C1_81 C2_81 C3_81 105.7(6) . . ? C2_81 C3_81 C4_81 105.4(7) . . ? O_81 C4_81 C3_81 104.8(7) . . ? C1_81 O_81 C4_81 100.4(11) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.313 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 605316' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H106 B2 Fe2 O P6' _chemical_formula_sum 'C54 H106 B2 Fe2 O P6' _chemical_formula_weight 1090.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.199(4) _cell_length_b 14.985(5) _cell_length_c 14.939(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.184(5) _cell_angle_gamma 90.00 _cell_volume 3094.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 457 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.76 _exptl_crystal_description Plate _exptl_crystal_colour Red/brown _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7743 _exptl_absorpt_correction_T_max 0.9554 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 5 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34755 _diffrn_reflns_av_R_equivalents 0.1619 _diffrn_reflns_av_sigmaI/netI 0.1833 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.05 _reflns_number_total 10679 _reflns_number_gt 5935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; The dataset is 97.4 % complete to theat = 25.24. The crystal is twinned with the relationship between the two components being a 179.9 degree rotation around the real axis; 1.000 -0.013 -0.919 (reciprocal axis; -0.993 0.006 1.000). Of the 457 reflections used to determine the unit-cell and twin relationship, 210 contribute to both domains, 152 to domain '1' only and 95 to domain '2' only. Attempts to integrate the data for each twin component separately were unsuccessful therefore the structure refinement was done versus data integrated as a single component. Another complicating factor is the overall poor quality of diffraction; less than 60% of the data exceed 2? and intensities are virtually non-existent at 2-theta angles greater than 40 degrees. The anisotropic displacement parameters for boron and carbon were restrained to simulate isotropic behavior using ISOR. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 10679 _refine_ls_number_parameters 610 _refine_ls_number_restraints 337 _refine_ls_R_factor_all 0.1702 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.533 _refine_ls_restrained_S_all 1.543 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.18067(11) 0.34922(8) 0.33441(10) 0.0339(4) Uani 1 1 d . . . Fe2 Fe 0.33389(11) 0.28816(9) 0.18497(10) 0.0343(4) Uani 1 1 d . . . P1 P 0.1387(2) 0.49468(17) 0.4017(2) 0.0338(8) Uani 1 1 d . . . P2 P 0.0101(2) 0.30750(16) 0.30569(19) 0.0337(8) Uani 1 1 d . . . P3 P 0.2169(2) 0.27611(18) 0.48629(19) 0.0332(7) Uani 1 1 d . . . P4 P 0.4019(2) 0.14134(17) 0.1436(2) 0.0341(8) Uani 1 1 d . . . P5 P 0.2961(2) 0.32810(17) 0.0201(2) 0.0361(8) Uani 1 1 d . . . P6 P 0.4891(2) 0.36798(17) 0.2119(2) 0.0356(8) Uani 1 1 d . . . O1 O 0.2522(5) 0.3176(5) 0.2558(5) 0.0410(19) Uani 1 1 d . . . B1 B 0.0298(8) 0.3728(8) 0.5040(8) 0.033(3) Uani 1 1 d U . . B2 B 0.5016(8) 0.2673(8) 0.0352(8) 0.031(3) Uani 1 1 d U . . C1 C -0.0330(6) 0.3801(6) 0.5803(6) 0.021(2) Uani 1 1 d U . . C2 C -0.1304(7) 0.3475(7) 0.5689(7) 0.039(3) Uani 1 1 d U . . H2 H -0.1626 0.3234 0.5112 0.046 Uiso 1 1 calc R . . C3 C -0.1780(8) 0.3503(7) 0.6397(7) 0.042(3) Uani 1 1 d U . . H3 H -0.2415 0.3264 0.6300 0.050 Uiso 1 1 calc R . . C4 C -0.1373(8) 0.3857(7) 0.7216(7) 0.040(3) Uani 1 1 d U . . H4 H -0.1715 0.3875 0.7693 0.048 Uiso 1 1 calc R . . C5 C -0.0466(8) 0.4189(7) 0.7352(8) 0.041(3) Uani 1 1 d U . . H5 H -0.0174 0.4456 0.7925 0.050 Uiso 1 1 calc R . . C6 C 0.0037(8) 0.4145(6) 0.6671(7) 0.030(3) Uani 1 1 d U . . H6 H 0.0682 0.4364 0.6806 0.036 Uiso 1 1 calc R . . C7 C 0.0446(7) 0.4761(6) 0.4657(7) 0.029(3) Uani 1 1 d U . . H7A H 0.0581 0.5166 0.5196 0.035 Uiso 1 1 calc R . . H7B H -0.0178 0.4950 0.4260 0.035 Uiso 1 1 calc R . . C8 C -0.0271(7) 0.3095(6) 0.4135(6) 0.038(3) Uani 1 1 d U . . H8A H -0.0960 0.3274 0.3992 0.045 Uiso 1 1 calc R . . H8B H -0.0247 0.2471 0.4357 0.045 Uiso 1 1 calc R . . C9 C 0.1418(7) 0.3244(7) 0.5561(7) 0.043(3) Uani 1 1 d U . . H9A H 0.1290 0.2771 0.5980 0.051 Uiso 1 1 calc R . . H9B H 0.1807 0.3708 0.5950 0.051 Uiso 1 1 calc R . . C10 C 0.2482(7) 0.5306(7) 0.4886(7) 0.034(3) Uani 1 1 d U . . H10 H 0.2716 0.4779 0.5285 0.040 Uiso 1 1 calc R . . C11 C 0.2284(8) 0.6086(7) 0.5534(8) 0.047(3) Uani 1 1 d U . . H11A H 0.1885 0.5861 0.5940 0.071 Uiso 1 1 calc R . . H11B H 0.1944 0.6574 0.5158 0.071 Uiso 1 1 calc R . . H11C H 0.2901 0.6306 0.5905 0.071 Uiso 1 1 calc R . . C12 C 0.3256(8) 0.5545(7) 0.4403(8) 0.046(3) Uani 1 1 d U . . H12A H 0.3117 0.6132 0.4114 0.069 Uiso 1 1 calc R . . H12B H 0.3278 0.5097 0.3931 0.069 Uiso 1 1 calc R . . H12C H 0.3881 0.5563 0.4847 0.069 Uiso 1 1 calc R . . C13 C 0.1073(7) 0.6026(6) 0.3313(7) 0.030(3) Uani 1 1 d U . . H13 H 0.1562 0.6486 0.3596 0.036 Uiso 1 1 calc R . . C14 C 0.0097(8) 0.6403(7) 0.3309(8) 0.047(3) Uani 1 1 d U . . H14A H 0.0047 0.7007 0.3051 0.070 Uiso 1 1 calc R . . H14B H 0.0006 0.6424 0.3939 0.070 Uiso 1 1 calc R . . H14C H -0.0403 0.6023 0.2933 0.070 Uiso 1 1 calc R . . C15 C 0.1170(9) 0.5888(7) 0.2303(8) 0.051(3) Uani 1 1 d U . . H15A H 0.0734 0.5409 0.2017 0.077 Uiso 1 1 calc R . . H15B H 0.1838 0.5726 0.2302 0.077 Uiso 1 1 calc R . . H15C H 0.0999 0.6442 0.1956 0.077 Uiso 1 1 calc R . . C16 C -0.0670(7) 0.3951(7) 0.2344(7) 0.038(3) Uani 1 1 d U . . H16 H -0.0355 0.4528 0.2580 0.045 Uiso 1 1 calc R . . C17 C -0.1712(8) 0.4057(8) 0.2421(8) 0.054(3) Uani 1 1 d U . . H17A H -0.2034 0.4505 0.1978 0.082 Uiso 1 1 calc R . . H17B H -0.1724 0.4251 0.3045 0.082 Uiso 1 1 calc R . . H17C H -0.2049 0.3485 0.2292 0.082 Uiso 1 1 calc R . . C18 C -0.0575(8) 0.3908(7) 0.1349(7) 0.046(3) Uani 1 1 d U . . H18A H -0.0916 0.3380 0.1051 0.070 Uiso 1 1 calc R . . H18B H 0.0110 0.3869 0.1335 0.070 Uiso 1 1 calc R . . H18C H -0.0858 0.4446 0.1022 0.070 Uiso 1 1 calc R . . C19 C -0.0268(8) 0.1937(7) 0.2582(7) 0.038(3) Uani 1 1 d U . . H19 H 0.0042 0.1497 0.3063 0.045 Uiso 1 1 calc R . . C20 C -0.1342(8) 0.1766(8) 0.2383(8) 0.061(4) Uani 1 1 d U . . H20A H -0.1646 0.2002 0.1774 0.091 Uiso 1 1 calc R . . H20B H -0.1618 0.2062 0.2849 0.091 Uiso 1 1 calc R . . H20C H -0.1460 0.1122 0.2396 0.091 Uiso 1 1 calc R . . C21 C 0.0130(8) 0.1745(7) 0.1724(7) 0.042(3) Uani 1 1 d U . . H21A H 0.0085 0.1104 0.1589 0.062 Uiso 1 1 calc R . . H21B H 0.0808 0.1933 0.1838 0.062 Uiso 1 1 calc R . . H21C H -0.0250 0.2076 0.1198 0.062 Uiso 1 1 calc R . . C22 C 0.1853(8) 0.1532(6) 0.4798(7) 0.033(3) Uani 1 1 d U . . H22 H 0.1130 0.1513 0.4647 0.040 Uiso 1 1 calc R . . C23 C 0.2165(8) 0.1033(7) 0.5722(8) 0.050(3) Uani 1 1 d U . . H23A H 0.1848 0.0449 0.5674 0.074 Uiso 1 1 calc R . . H23B H 0.1978 0.1382 0.6208 0.074 Uiso 1 1 calc R . . H23C H 0.2869 0.0952 0.5871 0.074 Uiso 1 1 calc R . . C24 C 0.2141(8) 0.1065(7) 0.4012(8) 0.046(3) Uani 1 1 d U . . H24A H 0.2843 0.0980 0.4157 0.069 Uiso 1 1 calc R . . H24B H 0.1947 0.1428 0.3454 0.069 Uiso 1 1 calc R . . H24C H 0.1819 0.0483 0.3912 0.069 Uiso 1 1 calc R . . C25 C 0.3439(8) 0.2863(9) 0.5536(7) 0.055(3) Uani 1 1 d U . . H25 H 0.3580 0.3503 0.5425 0.066 Uiso 1 1 calc R . . C26 C 0.3661(9) 0.2834(9) 0.6535(8) 0.065(4) Uani 1 1 d U . . H26A H 0.3627 0.2215 0.6738 0.098 Uiso 1 1 calc R . . H26B H 0.3191 0.3197 0.6762 0.098 Uiso 1 1 calc R . . H26C H 0.4313 0.3069 0.6777 0.098 Uiso 1 1 calc R . . C27 C 0.4160(9) 0.2398(8) 0.5115(8) 0.067(4) Uani 1 1 d U . . H27A H 0.4809 0.2630 0.5384 0.101 Uiso 1 1 calc R . . H27B H 0.4004 0.2504 0.4450 0.101 Uiso 1 1 calc R . . H27C H 0.4143 0.1756 0.5234 0.101 Uiso 1 1 calc R . . C28 C 0.5831(7) 0.2584(6) -0.0257(7) 0.029(3) Uani 1 1 d U . . C29 C 0.6738(7) 0.2173(6) 0.0129(7) 0.030(3) Uani 1 1 d U . . H29 H 0.6844 0.1906 0.0720 0.037 Uiso 1 1 calc R . . C30 C 0.7455(8) 0.2158(7) -0.0341(8) 0.042(3) Uani 1 1 d U . . H30 H 0.8051 0.1885 -0.0052 0.051 Uiso 1 1 calc R . . C31 C 0.7378(8) 0.2504(7) -0.1193(8) 0.042(3) Uani 1 1 d U . . H31 H 0.7907 0.2497 -0.1484 0.051 Uiso 1 1 calc R . . C32 C 0.6498(8) 0.2867(8) -0.1620(8) 0.044(3) Uani 1 1 d U . . H32 H 0.6395 0.3087 -0.2231 0.052 Uiso 1 1 calc R . . C33 C 0.5768(7) 0.2907(7) -0.1147(7) 0.033(3) Uani 1 1 d U . . H33 H 0.5175 0.3176 -0.1451 0.040 Uiso 1 1 calc R . . C34 C 0.4620(7) 0.1636(6) 0.0518(7) 0.029(3) Uani 1 1 d U . . H34A H 0.5186 0.1232 0.0607 0.035 Uiso 1 1 calc R . . H34B H 0.4172 0.1453 -0.0063 0.035 Uiso 1 1 calc R . . C35 C 0.4057(7) 0.3296(6) -0.0231(7) 0.037(3) Uani 1 1 d U . . H35A H 0.3891 0.3088 -0.0877 0.044 Uiso 1 1 calc R . . H35B H 0.4274 0.3923 -0.0237 0.044 Uiso 1 1 calc R . . C36 C 0.5575(7) 0.3196(7) 0.1350(6) 0.038(3) Uani 1 1 d U . . H36A H 0.5975 0.3680 0.1180 0.045 Uiso 1 1 calc R . . H36B H 0.6028 0.2758 0.1715 0.045 Uiso 1 1 calc R . . C37 C 0.5005(8) 0.1007(7) 0.2387(8) 0.044(3) Uani 1 1 d U . . H37 H 0.5470 0.1511 0.2572 0.053 Uiso 1 1 calc R . . C38 C 0.5575(8) 0.0214(7) 0.2178(8) 0.051(3) Uani 1 1 d U . . H38A H 0.6057 0.0045 0.2732 0.076 Uiso 1 1 calc R . . H38B H 0.5903 0.0372 0.1689 0.076 Uiso 1 1 calc R . . H38C H 0.5136 -0.0288 0.1976 0.076 Uiso 1 1 calc R . . C39 C 0.4555(8) 0.0797(7) 0.3218(8) 0.053(3) Uani 1 1 d U . . H39A H 0.4095 0.0302 0.3060 0.079 Uiso 1 1 calc R . . H39B H 0.4217 0.1326 0.3370 0.079 Uiso 1 1 calc R . . H39C H 0.5068 0.0629 0.3749 0.079 Uiso 1 1 calc R . . C40 C 0.3240(7) 0.0380(6) 0.1145(7) 0.026(2) Uani 1 1 d U . . H40 H 0.3539 -0.0087 0.1599 0.031 Uiso 1 1 calc R . . C41 C 0.3228(8) -0.0004(7) 0.0192(7) 0.044(3) Uani 1 1 d U . . H41A H 0.2898 -0.0583 0.0123 0.066 Uiso 1 1 calc R . . H41B H 0.3894 -0.0082 0.0125 0.066 Uiso 1 1 calc R . . H41C H 0.2885 0.0407 -0.0282 0.066 Uiso 1 1 calc R . . C42 C 0.2225(8) 0.0518(7) 0.1272(8) 0.043(3) Uani 1 1 d U . . H42A H 0.1937 0.1039 0.0916 0.065 Uiso 1 1 calc R . . H42B H 0.2246 0.0618 0.1925 0.065 Uiso 1 1 calc R . . H42C H 0.1834 -0.0012 0.1059 0.065 Uiso 1 1 calc R . . C43 C 0.2373(8) 0.4406(7) -0.0123(7) 0.035(3) Uani 1 1 d U . . H43 H 0.2881 0.4855 0.0143 0.042 Uiso 1 1 calc R . . C44 C 0.2146(10) 0.4572(8) -0.1145(8) 0.069(4) Uani 1 1 d U . . H44A H 0.1676 0.4129 -0.1456 0.104 Uiso 1 1 calc R . . H44B H 0.2741 0.4524 -0.1370 0.104 Uiso 1 1 calc R . . H44C H 0.1874 0.5172 -0.1273 0.104 Uiso 1 1 calc R . . C45 C 0.1567(8) 0.4595(7) 0.0306(8) 0.048(3) Uani 1 1 d U . . H45A H 0.1449 0.5240 0.0296 0.073 Uiso 1 1 calc R . . H45B H 0.1728 0.4385 0.0944 0.073 Uiso 1 1 calc R . . H45C H 0.0986 0.4288 -0.0033 0.073 Uiso 1 1 calc R . . C46 C 0.2164(8) 0.2411(7) -0.0498(7) 0.043(3) Uani 1 1 d U . . H46 H 0.2411 0.1833 -0.0202 0.052 Uiso 1 1 calc R . . C47 C 0.2255(9) 0.2317(8) -0.1471(8) 0.061(4) Uani 1 1 d U . . H47A H 0.1954 0.1757 -0.1727 0.092 Uiso 1 1 calc R . . H47B H 0.2941 0.2314 -0.1488 0.092 Uiso 1 1 calc R . . H47C H 0.1930 0.2819 -0.1835 0.092 Uiso 1 1 calc R . . C48 C 0.1136(8) 0.2451(7) -0.0415(8) 0.048(3) Uani 1 1 d U . . H48A H 0.0795 0.2924 -0.0814 0.071 Uiso 1 1 calc R . . H48B H 0.1117 0.2577 0.0224 0.071 Uiso 1 1 calc R . . H48C H 0.0821 0.1877 -0.0600 0.071 Uiso 1 1 calc R . . C49 C 0.4715(7) 0.4890(6) 0.1718(7) 0.035(3) Uani 1 1 d U . . H49 H 0.4515 0.4860 0.1032 0.042 Uiso 1 1 calc R . . C50 C 0.5643(8) 0.5450(7) 0.1930(8) 0.049(3) Uani 1 1 d U . . H50A H 0.5510 0.6040 0.1647 0.074 Uiso 1 1 calc R . . H50B H 0.6142 0.5151 0.1681 0.074 Uiso 1 1 calc R . . H50C H 0.5870 0.5516 0.2597 0.074 Uiso 1 1 calc R . . C51 C 0.3888(8) 0.5352(8) 0.2018(8) 0.052(3) Uani 1 1 d U . . H51A H 0.4092 0.5512 0.2669 0.078 Uiso 1 1 calc R . . H51B H 0.3331 0.4949 0.1927 0.078 Uiso 1 1 calc R . . H51C H 0.3709 0.5894 0.1651 0.078 Uiso 1 1 calc R . . C52 C 0.5766(9) 0.3828(8) 0.3244(8) 0.059(4) Uani 1 1 d U . . H52 H 0.6300 0.4212 0.3124 0.071 Uiso 1 1 calc R . . C53 C 0.6236(8) 0.2960(8) 0.3656(8) 0.062(3) Uani 1 1 d U . . H53A H 0.6742 0.3094 0.4205 0.093 Uiso 1 1 calc R . . H53B H 0.6522 0.2653 0.3203 0.093 Uiso 1 1 calc R . . H53C H 0.5745 0.2576 0.3825 0.093 Uiso 1 1 calc R . . C54 C 0.5322(9) 0.4332(8) 0.3945(8) 0.058(4) Uani 1 1 d U . . H54A H 0.4693 0.4070 0.3958 0.087 Uiso 1 1 calc R . . H54B H 0.5236 0.4962 0.3768 0.087 Uiso 1 1 calc R . . H54C H 0.5754 0.4285 0.4557 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0391(10) 0.0155(8) 0.0429(10) 0.0005(7) 0.0003(8) -0.0007(8) Fe2 0.0397(10) 0.0167(8) 0.0427(10) 0.0025(8) 0.0018(8) -0.0006(8) P1 0.0425(19) 0.0093(14) 0.0447(19) 0.0021(13) -0.0002(16) 0.0008(14) P2 0.0329(17) 0.0153(15) 0.0453(18) -0.0029(13) -0.0070(14) -0.0021(13) P3 0.0334(17) 0.0215(16) 0.0401(17) -0.0002(14) -0.0014(14) 0.0014(14) P4 0.0412(18) 0.0145(15) 0.0402(19) -0.0020(14) -0.0039(16) -0.0011(14) P5 0.0384(18) 0.0164(15) 0.0459(19) 0.0047(13) -0.0058(15) 0.0036(13) P6 0.0412(18) 0.0142(15) 0.0454(19) 0.0003(13) -0.0027(15) 0.0025(14) O1 0.028(4) 0.039(4) 0.043(4) 0.028(3) -0.021(3) -0.020(3) B1 0.029(5) 0.026(5) 0.039(5) 0.009(4) -0.003(4) -0.006(4) B2 0.032(5) 0.029(5) 0.028(5) 0.004(4) -0.002(4) -0.002(4) C1 0.020(4) 0.012(4) 0.027(4) 0.004(3) -0.004(3) 0.005(3) C2 0.039(5) 0.030(4) 0.044(5) -0.003(4) 0.004(4) 0.006(4) C3 0.047(5) 0.034(4) 0.046(5) 0.003(4) 0.013(4) -0.001(4) C4 0.047(5) 0.033(5) 0.043(5) 0.008(4) 0.015(4) 0.002(4) C5 0.049(5) 0.033(4) 0.040(5) 0.004(4) 0.005(4) 0.005(4) C6 0.030(4) 0.027(4) 0.031(4) 0.006(4) 0.004(4) 0.002(4) C7 0.030(4) 0.016(4) 0.033(4) -0.002(3) -0.011(3) 0.001(4) C8 0.041(4) 0.029(4) 0.039(4) -0.003(4) 0.000(4) 0.003(4) C9 0.046(5) 0.036(5) 0.042(5) 0.002(4) 0.002(4) -0.010(4) C10 0.037(5) 0.029(4) 0.033(4) 0.002(4) 0.006(4) 0.006(4) C11 0.045(5) 0.042(5) 0.051(5) -0.003(4) 0.003(4) 0.000(4) C12 0.044(5) 0.044(5) 0.045(5) 0.000(4) -0.001(4) 0.000(4) C13 0.031(4) 0.019(4) 0.038(5) 0.004(4) 0.003(4) -0.005(4) C14 0.051(5) 0.032(4) 0.053(5) 0.002(4) 0.004(4) -0.001(4) C15 0.054(5) 0.040(5) 0.057(5) 0.012(4) 0.007(4) -0.001(4) C16 0.041(5) 0.029(4) 0.041(5) 0.003(4) 0.004(4) -0.002(4) C17 0.050(5) 0.049(5) 0.062(5) 0.002(4) 0.007(4) 0.001(4) C18 0.052(5) 0.031(4) 0.051(5) 0.003(4) 0.001(4) -0.004(4) C19 0.042(5) 0.025(4) 0.044(5) -0.002(4) 0.007(4) 0.003(4) C20 0.063(5) 0.049(5) 0.068(5) -0.010(4) 0.010(4) -0.005(4) C21 0.048(5) 0.028(4) 0.045(5) -0.002(4) 0.003(4) 0.000(4) C22 0.037(4) 0.031(4) 0.031(4) 0.001(4) 0.007(4) -0.003(4) C23 0.052(5) 0.039(5) 0.056(5) 0.005(4) 0.007(4) -0.001(4) C24 0.051(5) 0.038(5) 0.048(5) 0.000(4) 0.008(4) -0.002(4) C25 0.057(5) 0.057(5) 0.049(5) 0.000(4) 0.011(4) 0.004(4) C26 0.063(5) 0.068(5) 0.063(5) 0.001(4) 0.008(4) 0.005(4) C27 0.067(5) 0.066(5) 0.064(5) -0.007(4) 0.006(4) 0.005(4) C28 0.028(4) 0.023(4) 0.029(4) -0.008(3) -0.003(4) -0.007(3) C29 0.027(4) 0.024(4) 0.038(4) 0.000(4) 0.002(4) -0.001(4) C30 0.044(5) 0.033(4) 0.048(5) -0.007(4) 0.006(4) -0.004(4) C31 0.045(5) 0.032(4) 0.049(5) -0.006(4) 0.009(4) -0.004(4) C32 0.051(5) 0.034(4) 0.046(5) -0.003(4) 0.012(4) -0.004(4) C33 0.040(4) 0.021(4) 0.036(4) -0.009(4) 0.002(4) -0.005(4) C34 0.030(4) 0.016(4) 0.034(4) -0.011(3) -0.008(4) -0.001(4) C35 0.045(5) 0.014(4) 0.045(4) -0.001(4) -0.004(4) 0.002(4) C36 0.037(4) 0.037(4) 0.036(4) 0.009(4) -0.001(4) 0.002(4) C37 0.045(5) 0.037(4) 0.048(5) -0.009(4) 0.003(4) -0.003(4) C38 0.049(5) 0.040(5) 0.060(5) 0.001(4) 0.004(4) 0.005(4) C39 0.057(5) 0.045(5) 0.052(5) 0.005(4) 0.003(4) -0.005(4) C40 0.029(4) 0.017(4) 0.029(4) -0.002(3) 0.003(4) -0.003(3) C41 0.041(5) 0.041(5) 0.046(5) 0.004(4) 0.001(4) -0.003(4) C42 0.051(5) 0.028(4) 0.048(5) 0.004(4) 0.005(4) -0.008(4) C43 0.041(5) 0.025(4) 0.037(5) 0.007(4) 0.004(4) -0.005(4) C44 0.072(6) 0.057(5) 0.072(6) -0.001(4) 0.004(4) -0.001(4) C45 0.049(5) 0.037(5) 0.055(5) -0.004(4) 0.005(4) 0.003(4) C46 0.049(5) 0.037(5) 0.042(5) 0.003(4) 0.007(4) -0.006(4) C47 0.064(5) 0.053(5) 0.060(5) -0.002(4) -0.002(4) -0.005(4) C48 0.049(5) 0.037(5) 0.052(5) -0.001(4) 0.000(4) 0.000(4) C49 0.034(4) 0.031(4) 0.037(4) -0.001(4) 0.003(4) 0.001(4) C50 0.050(5) 0.043(5) 0.053(5) -0.001(4) 0.008(4) -0.006(4) C51 0.054(5) 0.044(5) 0.057(5) -0.002(4) 0.010(4) -0.002(4) C52 0.064(5) 0.051(5) 0.066(5) 0.001(4) 0.022(4) 0.008(4) C53 0.063(5) 0.058(5) 0.059(5) -0.001(4) 0.002(4) 0.006(4) C54 0.062(5) 0.052(5) 0.057(5) 0.001(4) 0.006(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.783(8) . yes Fe1 P2 2.443(3) . yes Fe1 P3 2.466(3) . yes Fe1 P1 2.527(3) . yes Fe2 O1 1.795(8) . yes Fe2 P5 2.472(3) . yes Fe2 P6 2.459(3) . yes Fe2 P4 2.535(3) . yes P1 C7 1.834(11) . ? P1 C10 1.863(10) . ? P1 C13 1.926(10) . ? P2 C8 1.807(10) . ? P2 C19 1.875(10) . ? P2 C16 1.877(10) . ? P3 C9 1.804(11) . ? P3 C22 1.892(10) . ? P3 C25 1.860(11) . ? P4 C34 1.804(10) . ? P4 C37 1.855(11) . ? P4 C40 1.895(9) . ? P5 C35 1.816(10) . ? P5 C43 1.895(10) . ? P5 C46 1.879(11) . ? P6 C36 1.815(10) . ? P6 C49 1.908(10) . ? P6 C52 1.861(12) . ? B1 C1 1.604(15) . ? B1 C8 1.698(14) . ? B1 C7 1.680(14) . ? B1 C9 1.760(15) . ? B2 C28 1.632(15) . ? B2 C34 1.691(14) . ? B2 C36 1.710(14) . ? B2 C35 1.716(14) . ? C1 C6 1.382(12) . ? C1 C2 1.439(13) . ? C2 C3 1.379(13) . ? C3 C4 1.338(14) . ? C4 C5 1.352(14) . ? C5 C6 1.371(14) . ? C10 C12 1.488(14) . ? C10 C11 1.583(14) . ? C13 C14 1.495(14) . ? C13 C15 1.559(15) . ? C16 C18 1.524(13) . ? C16 C17 1.518(14) . ? C19 C20 1.508(15) . ? C19 C21 1.542(13) . ? C22 C24 1.502(14) . ? C22 C23 1.543(13) . ? C25 C26 1.453(14) . ? C25 C27 1.491(15) . ? C28 C33 1.398(13) . ? C28 C29 1.426(13) . ? C29 C30 1.363(14) . ? C30 C31 1.355(14) . ? C31 C32 1.378(14) . ? C32 C33 1.383(13) . ? C37 C39 1.553(15) . ? C37 C38 1.509(14) . ? C40 C41 1.532(13) . ? C40 C42 1.510(13) . ? C43 C45 1.461(14) . ? C43 C44 1.507(14) . ? C46 C48 1.494(14) . ? C46 C47 1.494(14) . ? C49 C50 1.533(13) . ? C49 C51 1.516(14) . ? C52 C53 1.525(15) . ? C52 C54 1.539(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 P2 120.5(2) . . yes O1 Fe1 P3 117.2(2) . . yes P2 Fe1 P3 92.19(11) . . yes O1 Fe1 P1 135.4(2) . . yes P2 Fe1 P1 88.65(10) . . yes P3 Fe1 P1 92.06(11) . . yes O1 Fe2 P5 120.4(2) . . yes O1 Fe2 P6 117.4(2) . . yes P5 Fe2 P6 91.59(11) . . yes O1 Fe2 P4 133.7(2) . . yes P5 Fe2 P4 88.59(10) . . yes P6 Fe2 P4 94.87(10) . . yes C7 P1 C10 105.8(5) . . ? C7 P1 C13 107.9(4) . . ? C10 P1 C13 101.0(5) . . ? C7 P1 Fe1 110.0(3) . . ? C10 P1 Fe1 107.0(3) . . ? C13 P1 Fe1 123.6(3) . . ? C8 P2 C19 103.8(5) . . ? C8 P2 C16 104.1(5) . . ? C19 P2 C16 110.2(5) . . ? C8 P2 Fe1 108.6(3) . . ? C19 P2 Fe1 118.6(4) . . ? C16 P2 Fe1 110.3(3) . . ? C9 P3 C22 104.8(5) . . ? C9 P3 C25 106.4(5) . . ? C22 P3 C25 107.3(5) . . ? C9 P3 Fe1 109.1(3) . . ? C22 P3 Fe1 112.8(3) . . ? C25 P3 Fe1 115.7(4) . . ? C34 P4 C37 103.7(5) . . ? C34 P4 C40 109.2(4) . . ? C37 P4 C40 101.9(5) . . ? C34 P4 Fe2 107.3(3) . . ? C37 P4 Fe2 111.2(4) . . ? C40 P4 Fe2 122.0(3) . . ? C35 P5 C43 105.2(5) . . ? C35 P5 C46 105.5(5) . . ? C43 P5 C46 107.5(5) . . ? C35 P5 Fe2 110.4(3) . . ? C43 P5 Fe2 116.9(3) . . ? C46 P5 Fe2 110.6(4) . . ? C36 P6 C49 103.4(5) . . ? C36 P6 C52 106.0(5) . . ? C49 P6 C52 100.5(5) . . ? C36 P6 Fe2 106.9(3) . . ? C49 P6 Fe2 111.2(3) . . ? C52 P6 Fe2 126.5(4) . . ? Fe2 O1 Fe1 174.7(4) . . ? C1 B1 C8 111.3(8) . . ? C1 B1 C7 108.2(8) . . ? C8 B1 C7 108.5(8) . . ? C1 B1 C9 107.9(8) . . ? C8 B1 C9 109.8(8) . . ? C7 B1 C9 111.1(8) . . ? C28 B2 C34 108.0(8) . . ? C28 B2 C36 106.1(8) . . ? C34 B2 C36 113.4(8) . . ? C28 B2 C35 110.1(8) . . ? C34 B2 C35 108.8(8) . . ? C36 B2 C35 110.5(8) . . ? C6 C1 C2 112.6(9) . . ? C6 C1 B1 122.7(9) . . ? C2 C1 B1 124.6(8) . . ? C3 C2 C1 121.6(10) . . ? C4 C3 C2 121.9(11) . . ? C3 C4 C5 118.7(11) . . ? C4 C5 C6 120.7(11) . . ? C1 C6 C5 124.4(10) . . ? B1 C7 P1 118.7(7) . . ? B1 C8 P2 122.4(7) . . ? B1 C9 P3 120.2(7) . . ? C12 C10 C11 111.9(9) . . ? C12 C10 P1 108.8(7) . . ? C11 C10 P1 113.8(7) . . ? C14 C13 C15 109.4(9) . . ? C14 C13 P1 114.7(7) . . ? C15 C13 P1 110.8(7) . . ? C18 C16 C17 112.6(9) . . ? C18 C16 P2 110.7(7) . . ? C17 C16 P2 118.8(8) . . ? C20 C19 C21 110.5(9) . . ? C20 C19 P2 114.3(8) . . ? C21 C19 P2 111.1(7) . . ? C24 C22 C23 113.6(9) . . ? C24 C22 P3 112.9(7) . . ? C23 C22 P3 114.2(7) . . ? C26 C25 C27 114.2(10) . . ? C26 C25 P3 120.6(8) . . ? C27 C25 P3 114.1(8) . . ? C33 C28 C29 113.0(9) . . ? C33 C28 B2 127.0(9) . . ? C29 C28 B2 120.0(9) . . ? C30 C29 C28 120.7(10) . . ? C29 C30 C31 124.6(11) . . ? C32 C31 C30 117.1(11) . . ? C31 C32 C33 119.2(11) . . ? C32 C33 C28 125.3(10) . . ? B2 C34 P4 120.8(7) . . ? B2 C35 P5 117.3(7) . . ? B2 C36 P6 121.8(7) . . ? C39 C37 C38 110.1(10) . . ? C39 C37 P4 107.6(8) . . ? C38 C37 P4 116.6(8) . . ? C41 C40 C42 111.1(9) . . ? C41 C40 P4 113.7(7) . . ? C42 C40 P4 112.5(7) . . ? C45 C43 C44 113.9(10) . . ? C45 C43 P5 113.8(7) . . ? C44 C43 P5 112.7(8) . . ? C48 C46 C47 112.8(10) . . ? C48 C46 P5 113.7(8) . . ? C47 C46 P5 115.5(8) . . ? C50 C49 C51 112.0(9) . . ? C50 C49 P6 114.2(7) . . ? C51 C49 P6 113.3(7) . . ? C53 C52 C54 110.6(10) . . ? C53 C52 P6 113.8(8) . . ? C54 C52 P6 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.317 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.127 _database_code_depnum_ccdc_archive 'CCDC 626195' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H82 B2 FE2 O P6, 2(C6 H6)' _chemical_formula_sum 'C102 H94 B2 Fe2 O P6' _chemical_formula_weight 1654.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I -4 2 d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 33.2834(6) _cell_length_b 33.2834(6) _cell_length_c 16.7509(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18556.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.38 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6928 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8367 _exptl_absorpt_correction_T_max 0.8738 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 124894 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.61 _reflns_number_total 8762 _reflns_number_gt 8196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT 7 (Bruker-AXS, 2005)' _computing_data_reduction 'SAINT 7 (Bruker-AXS, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+24.5799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(18) _refine_ls_number_reflns 8762 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 4119 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.42058(15) 0.7500 0.1250 0.0608(11) Uani 1 2 d SU . . Fe1 Fe 0.405949(14) 0.768989(15) 0.03185(3) 0.03532(14) Uani 1 1 d U A . P1 P 0.42778(3) 0.83411(3) -0.01088(5) 0.0404(2) Uani 1 1 d DU . . C10 C 0.4782(2) 0.8483(3) 0.0219(6) 0.0500(19) Uani 0.59(2) 1 d PDU A 1 C11 C 0.5006(4) 0.8770(4) -0.0169(9) 0.064(3) Uani 0.59(2) 1 d PDU A 1 H11 H 0.4895 0.8909 -0.0613 0.077 Uiso 0.59(2) 1 calc PR A 1 C12 C 0.5394(4) 0.8857(5) 0.0085(9) 0.065(3) Uani 0.59(2) 1 d PDU A 1 H12 H 0.5551 0.9048 -0.0198 0.078 Uiso 0.59(2) 1 calc PR A 1 C13 C 0.5552(4) 0.8669(5) 0.0740(8) 0.072(3) Uani 0.59(2) 1 d PDU A 1 H13 H 0.5815 0.8735 0.0915 0.086 Uiso 0.59(2) 1 calc PR A 1 C14 C 0.5336(3) 0.8389(4) 0.1141(8) 0.071(3) Uani 0.59(2) 1 d PDU A 1 H14 H 0.5445 0.8263 0.1602 0.085 Uiso 0.59(2) 1 calc PR A 1 C15 C 0.4958(3) 0.8289(4) 0.0871(7) 0.054(2) Uani 0.59(2) 1 d PDU A 1 H15 H 0.4813 0.8082 0.1136 0.065 Uiso 0.59(2) 1 calc PR A 1 C10A C 0.4768(3) 0.8493(3) 0.0289(9) 0.046(2) Uani 0.41(2) 1 d PDU A 2 C11A C 0.5058(5) 0.8679(7) -0.0155(11) 0.059(3) Uani 0.41(2) 1 d PDU A 2 H11A H 0.5010 0.8738 -0.0702 0.071 Uiso 0.41(2) 1 calc PR A 2 C12A C 0.5423(6) 0.8783(8) 0.0195(14) 0.067(3) Uani 0.41(2) 1 d PDU A 2 H12A H 0.5620 0.8918 -0.0116 0.080 Uiso 0.41(2) 1 calc PR A 2 C13A C 0.5505(5) 0.8696(7) 0.0965(13) 0.071(3) Uani 0.41(2) 1 d PDU A 2 H13A H 0.5759 0.8759 0.1191 0.085 Uiso 0.41(2) 1 calc PR A 2 C14A C 0.5214(5) 0.8516(6) 0.1406(11) 0.071(3) Uani 0.41(2) 1 d PDU A 2 H14A H 0.5264 0.8459 0.1953 0.085 Uiso 0.41(2) 1 calc PR A 2 C15A C 0.4849(5) 0.8416(6) 0.1084(9) 0.060(3) Uani 0.41(2) 1 d PDU A 2 H15A H 0.4651 0.8291 0.1408 0.072 Uiso 0.41(2) 1 calc PR A 2 C16 C 0.3952(3) 0.8752(3) 0.0201(5) 0.0488(19) Uani 0.502(4) 1 d PDU A 1 C17 C 0.3661(3) 0.8673(3) 0.0765(5) 0.066(2) Uani 0.502(4) 1 d PDU A 1 H17 H 0.3628 0.8409 0.0967 0.080 Uiso 0.502(4) 1 calc PR A 1 C18 C 0.3419(4) 0.8982(3) 0.1037(7) 0.084(3) Uani 0.502(4) 1 d PDU A 1 H18 H 0.3229 0.8929 0.1446 0.101 Uiso 0.502(4) 1 calc PR A 1 C19 C 0.3447(4) 0.9356(4) 0.0734(9) 0.085(3) Uani 0.502(4) 1 d PDU A 1 H19 H 0.3278 0.9565 0.0925 0.102 Uiso 0.502(4) 1 calc PR A 1 C20 C 0.3722(4) 0.9429(3) 0.0149(8) 0.094(3) Uani 0.502(4) 1 d PDU A 1 H20 H 0.3738 0.9689 -0.0082 0.113 Uiso 0.502(4) 1 calc PR A 1 C21 C 0.3980(4) 0.9129(2) -0.0114(7) 0.076(3) Uani 0.502(4) 1 d PDU A 1 H21 H 0.4175 0.9186 -0.0512 0.091 Uiso 0.502(4) 1 calc PR A 1 C16A C 0.3972(2) 0.8760(2) 0.0342(6) 0.0496(19) Uani 0.498(4) 1 d PDU A 2 C17A C 0.3727(3) 0.9007(3) -0.0103(6) 0.066(2) Uani 0.498(4) 1 d PDU A 2 H17A H 0.3730 0.8993 -0.0670 0.079 Uiso 0.498(4) 1 calc PR A 2 C18A C 0.3477(4) 0.9275(4) 0.0282(8) 0.084(3) Uani 0.498(4) 1 d PDU A 2 H18A H 0.3273 0.9408 -0.0015 0.101 Uiso 0.498(4) 1 calc PR A 2 C19A C 0.3516(4) 0.9355(4) 0.1086(7) 0.073(3) Uani 0.498(4) 1 d PDU A 2 H19A H 0.3358 0.9558 0.1330 0.088 Uiso 0.498(4) 1 calc PR A 2 C20A C 0.3781(3) 0.9140(3) 0.1524(6) 0.069(2) Uani 0.498(4) 1 d PDU A 2 H20A H 0.3813 0.9194 0.2077 0.083 Uiso 0.498(4) 1 calc PR A 2 C21A C 0.4007(3) 0.8841(3) 0.1162(5) 0.0580(19) Uani 0.498(4) 1 d PDU A 2 H21A H 0.4189 0.8687 0.1476 0.070 Uiso 0.498(4) 1 calc PR A 2 P2 P 0.43883(3) 0.74047(3) -0.08215(6) 0.0382(2) Uani 1 1 d DU . . C22 C 0.49237(19) 0.75361(19) -0.0814(5) 0.0435(15) Uani 0.665(19) 1 d PDU A 1 C23 C 0.5136(2) 0.7621(3) -0.1495(5) 0.0571(19) Uani 0.665(19) 1 d PDU A 1 H23 H 0.5005 0.7619 -0.1999 0.069 Uiso 0.665(19) 1 calc PR A 1 C24 C 0.5543(3) 0.7710(4) -0.1449(6) 0.072(2) Uani 0.665(19) 1 d PDU A 1 H24 H 0.5690 0.7762 -0.1924 0.086 Uiso 0.665(19) 1 calc PR A 1 C25 C 0.5732(3) 0.7722(4) -0.0733(7) 0.076(2) Uani 0.665(19) 1 d PDU A 1 H25 H 0.6007 0.7797 -0.0702 0.091 Uiso 0.665(19) 1 calc PR A 1 C26 C 0.5522(3) 0.7624(4) -0.0049(6) 0.075(2) Uani 0.665(19) 1 d PDU A 1 H26 H 0.5659 0.7616 0.0449 0.090 Uiso 0.665(19) 1 calc PR A 1 C27 C 0.5116(2) 0.7539(3) -0.0081(5) 0.054(2) Uani 0.665(19) 1 d PDU A 1 H27 H 0.4971 0.7482 0.0395 0.065 Uiso 0.665(19) 1 calc PR A 1 C22A C 0.4926(3) 0.7519(3) -0.0753(9) 0.045(3) Uani 0.335(19) 1 d PDU A 2 C23A C 0.5144(5) 0.7745(6) -0.1287(12) 0.064(3) Uani 0.335(19) 1 d PDU A 2 H23A H 0.5015 0.7858 -0.1740 0.077 Uiso 0.335(19) 1 calc PR A 2 C24A C 0.5552(5) 0.7807(6) -0.1165(14) 0.073(4) Uani 0.335(19) 1 d PDU A 2 H24A H 0.5693 0.7970 -0.1536 0.087 Uiso 0.335(19) 1 calc PR A 2 C25A C 0.5760(6) 0.7646(8) -0.0539(14) 0.078(4) Uani 0.335(19) 1 d PDU A 2 H25A H 0.6041 0.7687 -0.0476 0.093 Uiso 0.335(19) 1 calc PR A 2 C26A C 0.5544(4) 0.7427(7) -0.0017(11) 0.067(3) Uani 0.335(19) 1 d PDU A 2 H26A H 0.5678 0.7305 0.0421 0.080 Uiso 0.335(19) 1 calc PR A 2 C27A C 0.5134(4) 0.7373(7) -0.0096(10) 0.056(3) Uani 0.335(19) 1 d PDU A 2 H27A H 0.4992 0.7233 0.0309 0.068 Uiso 0.335(19) 1 calc PR A 2 C28 C 0.4454(2) 0.6860(2) -0.1019(5) 0.0469(17) Uani 0.577(8) 1 d PDU A 1 C29 C 0.4561(3) 0.6614(2) -0.0384(5) 0.076(2) Uani 0.577(8) 1 d PDU A 1 H29 H 0.4576 0.6726 0.0137 0.091 Uiso 0.577(8) 1 calc PR A 1 C30 C 0.4646(4) 0.6212(3) -0.0488(6) 0.087(3) Uani 0.577(8) 1 d PDU A 1 H30 H 0.4741 0.6058 -0.0049 0.104 Uiso 0.577(8) 1 calc PR A 1 C31 C 0.4598(3) 0.6036(3) -0.1202(6) 0.073(2) Uani 0.577(8) 1 d PDU A 1 H31 H 0.4635 0.5755 -0.1266 0.087 Uiso 0.577(8) 1 calc PR A 1 C32 C 0.4495(3) 0.6269(3) -0.1823(6) 0.071(2) Uani 0.577(8) 1 d PDU A 1 H32 H 0.4469 0.6149 -0.2334 0.085 Uiso 0.577(8) 1 calc PR A 1 C33 C 0.4426(3) 0.6676(2) -0.1749(5) 0.061(2) Uani 0.577(8) 1 d PDU A 1 H33 H 0.4358 0.6830 -0.2207 0.074 Uiso 0.577(8) 1 calc PR A 1 C28A C 0.4389(3) 0.6859(3) -0.0844(6) 0.047(2) Uani 0.423(8) 1 d PDU A 2 C29A C 0.4202(4) 0.6635(3) -0.0268(7) 0.077(3) Uani 0.423(8) 1 d PDU A 2 H29A H 0.4055 0.6764 0.0145 0.093 Uiso 0.423(8) 1 calc PR A 2 C30A C 0.4228(6) 0.6220(3) -0.0288(9) 0.104(4) Uani 0.423(8) 1 d PDU A 2 H30A H 0.4103 0.6066 0.0121 0.125 Uiso 0.423(8) 1 calc PR A 2 C31A C 0.4428(5) 0.6031(4) -0.0882(9) 0.090(3) Uani 0.423(8) 1 d PDU A 2 H31A H 0.4447 0.5746 -0.0887 0.108 Uiso 0.423(8) 1 calc PR A 2 C32A C 0.4599(5) 0.6249(4) -0.1462(9) 0.075(3) Uani 0.423(8) 1 d PDU A 2 H32A H 0.4743 0.6116 -0.1874 0.091 Uiso 0.423(8) 1 calc PR A 2 C33A C 0.4571(4) 0.6668(3) -0.1474(8) 0.067(3) Uani 0.423(8) 1 d PDU A 2 H33A H 0.4675 0.6817 -0.1910 0.080 Uiso 0.423(8) 1 calc PR A 2 P3 P 0.34361(3) 0.77372(3) -0.04068(5) 0.0365(2) Uani 1 1 d DU . . C34 C 0.32856(17) 0.72534(16) -0.0839(4) 0.0361(12) Uani 0.675(7) 1 d PDU A 1 C35 C 0.3394(2) 0.69020(16) -0.0451(4) 0.0540(15) Uani 0.675(7) 1 d PDU A 1 H35 H 0.3542 0.6919 0.0033 0.065 Uiso 0.675(7) 1 calc PR A 1 C36 C 0.3293(2) 0.65252(18) -0.0748(5) 0.0654(18) Uani 0.675(7) 1 d PDU A 1 H36 H 0.3377 0.6290 -0.0475 0.078 Uiso 0.675(7) 1 calc PR A 1 C37 C 0.3075(2) 0.6494(2) -0.1424(4) 0.0557(16) Uani 0.675(7) 1 d PDU A 1 H37 H 0.2998 0.6237 -0.1619 0.067 Uiso 0.675(7) 1 calc PR A 1 C38 C 0.2965(3) 0.6834(2) -0.1826(4) 0.065(2) Uani 0.675(7) 1 d PDU A 1 H38 H 0.2813 0.6811 -0.2305 0.078 Uiso 0.675(7) 1 calc PR A 1 C39 C 0.3072(3) 0.7216(2) -0.1547(4) 0.0574(19) Uani 0.675(7) 1 d PDU A 1 H39 H 0.2999 0.7449 -0.1842 0.069 Uiso 0.675(7) 1 calc PR A 1 C34A C 0.3249(3) 0.7240(3) -0.0643(7) 0.045(2) Uani 0.325(7) 1 d PDU A 2 C35A C 0.3122(4) 0.7000(3) -0.0033(7) 0.058(3) Uani 0.325(7) 1 d PDU A 2 H35A H 0.3132 0.7089 0.0506 0.069 Uiso 0.325(7) 1 calc PR A 2 C36A C 0.2978(5) 0.6625(4) -0.0224(9) 0.077(3) Uani 0.325(7) 1 d PDU A 2 H36A H 0.2880 0.6457 0.0190 0.092 Uiso 0.325(7) 1 calc PR A 2 C37A C 0.2973(6) 0.6490(4) -0.0980(10) 0.076(3) Uani 0.325(7) 1 d PDU A 2 H37A H 0.2882 0.6225 -0.1088 0.091 Uiso 0.325(7) 1 calc PR A 2 C38A C 0.3095(5) 0.6726(5) -0.1587(10) 0.063(3) Uani 0.325(7) 1 d PDU A 2 H38A H 0.3095 0.6627 -0.2118 0.076 Uiso 0.325(7) 1 calc PR A 2 C39A C 0.3221(4) 0.7118(4) -0.1429(8) 0.049(3) Uani 0.325(7) 1 d PDU A 2 H39A H 0.3285 0.7296 -0.1852 0.059 Uiso 0.325(7) 1 calc PR A 2 C40 C 0.2949(2) 0.7898(3) 0.0008(5) 0.0475(19) Uani 0.502(4) 1 d PDU A 1 C41 C 0.2757(3) 0.8244(3) -0.0219(7) 0.088(3) Uani 0.502(4) 1 d PDU A 1 H41 H 0.2868 0.8406 -0.0629 0.106 Uiso 0.502(4) 1 calc PR A 1 C42 C 0.2398(3) 0.8358(4) 0.0151(7) 0.086(3) Uani 0.502(4) 1 d PDU A 1 H42 H 0.2277 0.8605 -0.0003 0.103 Uiso 0.502(4) 1 calc PR A 1 C43 C 0.2217(3) 0.8134(3) 0.0716(7) 0.079(3) Uani 0.502(4) 1 d PDU A 1 H43 H 0.1993 0.8230 0.1010 0.095 Uiso 0.502(4) 1 calc PR A 1 C44 C 0.2374(3) 0.7763(4) 0.0840(8) 0.098(3) Uani 0.502(4) 1 d PDU A 1 H44 H 0.2231 0.7580 0.1170 0.117 Uiso 0.502(4) 1 calc PR A 1 C45 C 0.2736(3) 0.7640(3) 0.0502(7) 0.083(3) Uani 0.502(4) 1 d PDU A 1 H45 H 0.2838 0.7378 0.0610 0.099 Uiso 0.502(4) 1 calc PR A 1 C40A C 0.3015(3) 0.7962(3) 0.0136(5) 0.0533(19) Uani 0.498(4) 1 d PDU A 2 C41A C 0.2619(2) 0.7889(4) -0.0051(7) 0.085(3) Uani 0.498(4) 1 d PDU A 2 H41A H 0.2556 0.7716 -0.0483 0.101 Uiso 0.498(4) 1 calc PR A 2 C42A C 0.2310(3) 0.8068(5) 0.0386(8) 0.097(3) Uani 0.498(4) 1 d PDU A 2 H42A H 0.2039 0.7990 0.0296 0.117 Uiso 0.498(4) 1 calc PR A 2 C43A C 0.2396(3) 0.8349(4) 0.0932(7) 0.086(3) Uani 0.498(4) 1 d PDU A 2 H43A H 0.2187 0.8514 0.1139 0.103 Uiso 0.498(4) 1 calc PR A 2 C44A C 0.2774(3) 0.8401(4) 0.1190(6) 0.074(3) Uani 0.498(4) 1 d PDU A 2 H44A H 0.2829 0.8569 0.1636 0.088 Uiso 0.498(4) 1 calc PR A 2 C45A C 0.3084(2) 0.8205(3) 0.0793(5) 0.057(2) Uani 0.498(4) 1 d PDU A 2 H45A H 0.3352 0.8239 0.0978 0.069 Uiso 0.498(4) 1 calc PR A 2 C7 C 0.42862(13) 0.83781(12) -0.1195(2) 0.0451(8) Uani 1 1 d U A . H7A H 0.4217 0.8657 -0.1345 0.054 Uiso 1 1 calc R . . H7B H 0.4564 0.8327 -0.1379 0.054 Uiso 1 1 calc R . . C8 C 0.41809(11) 0.76103(12) -0.1737(2) 0.0391(7) Uani 1 1 d U A . H8A H 0.4397 0.7615 -0.2144 0.047 Uiso 1 1 calc R . . H8B H 0.3970 0.7425 -0.1931 0.047 Uiso 1 1 calc R . . C9 C 0.35239(11) 0.80626(11) -0.1264(2) 0.0411(7) Uani 1 1 d U A . H9A H 0.3330 0.7985 -0.1685 0.049 Uiso 1 1 calc R . . H9B H 0.3457 0.8341 -0.1101 0.049 Uiso 1 1 calc R . . B1 B 0.39823(12) 0.80718(13) -0.1682(2) 0.0380(8) Uani 1 1 d DU . . C1 C 0.38958(12) 0.82497(12) -0.2584(2) 0.0458(8) Uani 1 1 d DU A . C2 C 0.3881(2) 0.80174(16) -0.3254(3) 0.0784(16) Uani 1 1 d DU . . H2 H 0.3945 0.7740 -0.3208 0.094 Uiso 1 1 calc R A . C3 C 0.3778(2) 0.81649(19) -0.3997(3) 0.0864(18) Uani 1 1 d DU A . H3 H 0.3759 0.7985 -0.4436 0.104 Uiso 1 1 calc R . . C4 C 0.37051(19) 0.85598(17) -0.4111(3) 0.0739(14) Uani 1 1 d DU . . H4 H 0.3665 0.8664 -0.4633 0.089 Uiso 1 1 calc R A . C5 C 0.36896(19) 0.88089(16) -0.3453(3) 0.0732(14) Uani 1 1 d DU A . H5 H 0.3618 0.9084 -0.3509 0.088 Uiso 1 1 calc R . . C6 C 0.37813(17) 0.86493(15) -0.2699(3) 0.0673(12) Uani 1 1 d DU . . H6 H 0.3765 0.8821 -0.2246 0.081 Uiso 1 1 calc R A . C1S C 0.4272(4) 1.0080(3) 0.8867(7) 0.114(4) Uani 0.50 1 d PDU . . H1S H 0.4405 1.0188 0.9321 0.136 Uiso 0.50 1 calc PR . . C2S C 0.3914(4) 1.0232(3) 0.8642(7) 0.116(4) Uani 0.50 1 d PDU . . H2S H 0.3796 1.0445 0.8939 0.140 Uiso 0.50 1 calc PR . . C3S C 0.3723(4) 1.0083(3) 0.8001(7) 0.111(4) Uani 0.50 1 d PDU . . H3S H 0.3471 1.0189 0.7840 0.133 Uiso 0.50 1 calc PR . . C4S C 0.3892(4) 0.9783(4) 0.7592(7) 0.117(4) Uani 0.50 1 d PDU . . H4S H 0.3758 0.9674 0.7141 0.141 Uiso 0.50 1 calc PR . . C5S C 0.4251(4) 0.9633(3) 0.7809(7) 0.108(4) Uani 0.50 1 d PDU . . H5S H 0.4370 0.9423 0.7505 0.130 Uiso 0.50 1 calc PR . . C6S C 0.4442(4) 0.9779(3) 0.8456(7) 0.108(4) Uani 0.50 1 d PDU . . H6S H 0.4692 0.9670 0.8618 0.129 Uiso 0.50 1 calc PR . . C1T C 0.5440(8) 0.7126(7) 0.6208(18) 0.075(6) Uani 0.153(6) 1 d PDU B -1 H1T H 0.5503 0.6848 0.6234 0.090 Uiso 0.153(6) 1 calc PR B -1 C2T C 0.5055(8) 0.7247(8) 0.6183(17) 0.071(6) Uani 0.153(6) 1 d PDU B -1 H2T H 0.4845 0.7054 0.6190 0.085 Uiso 0.153(6) 1 calc PR B -1 C3T C 0.4967(7) 0.7640(8) 0.6149(17) 0.066(5) Uani 0.153(6) 1 d PDU B -1 H3T H 0.4695 0.7725 0.6134 0.079 Uiso 0.153(6) 1 calc PR B -1 C4T C 0.5262(7) 0.7915(7) 0.6136(15) 0.072(5) Uani 0.153(6) 1 d PDU B -1 H4T H 0.5200 0.8193 0.6104 0.086 Uiso 0.153(6) 1 calc PR B -1 C5T C 0.5648(7) 0.7794(7) 0.6168(16) 0.074(5) Uani 0.153(6) 1 d PDU B -1 H5T H 0.5858 0.7987 0.6171 0.089 Uiso 0.153(6) 1 calc PR B -1 C6T C 0.5735(7) 0.7400(7) 0.620(2) 0.080(6) Uani 0.153(6) 1 d PDU B -1 H6T H 0.6008 0.7316 0.6209 0.096 Uiso 0.153(6) 1 calc PR B -1 C1TA C 0.5358(12) 0.7314(11) 0.615(2) 0.068(5) Uani 0.097(6) 1 d PDU B -2 H1TA H 0.5433 0.7047 0.6017 0.082 Uiso 0.097(6) 1 calc PR B -2 C2TA C 0.4973(11) 0.7428(12) 0.6095(19) 0.067(6) Uani 0.097(6) 1 d PDU B -2 H2TA H 0.4775 0.7243 0.5916 0.080 Uiso 0.097(6) 1 calc PR B -2 C3TA C 0.4869(10) 0.7805(13) 0.6290(18) 0.069(6) Uani 0.097(6) 1 d PDU B -2 H3TA H 0.4596 0.7887 0.6249 0.083 Uiso 0.097(6) 1 calc PR B -2 C4TA C 0.5147(12) 0.8067(10) 0.6544(19) 0.073(6) Uani 0.097(6) 1 d PDU B -2 H4TA H 0.5072 0.8333 0.6681 0.088 Uiso 0.097(6) 1 calc PR B -2 C5TA C 0.5534(11) 0.7952(11) 0.660(2) 0.071(6) Uani 0.097(6) 1 d PDU B -2 H5TA H 0.5732 0.8137 0.6781 0.085 Uiso 0.097(6) 1 calc PR B -2 C6TA C 0.5638(10) 0.7575(13) 0.641(2) 0.074(6) Uani 0.097(6) 1 d PDU B -2 H6TA H 0.5911 0.7492 0.6449 0.089 Uiso 0.097(6) 1 calc PR B -2 C1U C 0.5015(9) 1.0245(9) 0.2043(11) 0.109(7) Uani 0.25 1 d PDU C -1 H1U H 0.5025 1.0382 0.2540 0.131 Uiso 0.25 1 calc PR C -1 C2U C 0.5175(7) 1.0416(7) 0.1389(15) 0.096(6) Uani 0.25 1 d PDU C -1 H2U H 0.5300 1.0672 0.1424 0.115 Uiso 0.25 1 calc PR C -1 C3U C 0.5159(8) 1.0222(8) 0.0688(12) 0.085(6) Uani 0.25 1 d PDU C -1 H3U H 0.5272 1.0342 0.0225 0.102 Uiso 0.25 1 calc PR C -1 C4U C 0.4983(8) 0.9859(9) 0.0637(11) 0.083(6) Uani 0.25 1 d PDU C -1 H4U H 0.4973 0.9724 0.0138 0.099 Uiso 0.25 1 calc PR C -1 C5U C 0.4822(7) 0.9688(8) 0.1286(15) 0.098(6) Uani 0.25 1 d PDU C -1 H5U H 0.4696 0.9433 0.1248 0.118 Uiso 0.25 1 calc PR C -1 C6U C 0.4840(8) 0.9880(9) 0.1994(12) 0.104(6) Uani 0.25 1 d PDU C -1 H6U H 0.4729 0.9759 0.2458 0.125 Uiso 0.25 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.078(3) 0.067(3) 0.0370(18) 0.0152(18) 0.000 0.000 Fe1 0.0340(3) 0.0412(3) 0.0308(2) 0.00147(19) -0.00106(19) 0.0033(2) P1 0.0467(5) 0.0415(5) 0.0331(4) 0.0045(4) -0.0059(4) -0.0069(4) C10 0.056(3) 0.048(4) 0.046(4) 0.004(4) -0.008(3) -0.013(3) C11 0.057(4) 0.068(6) 0.067(5) 0.019(4) -0.014(4) -0.016(4) C12 0.055(4) 0.074(6) 0.066(5) 0.003(4) -0.004(4) -0.016(4) C13 0.059(5) 0.088(6) 0.067(6) 0.006(5) -0.017(4) -0.025(4) C14 0.052(4) 0.093(6) 0.067(6) 0.015(4) -0.014(4) -0.010(4) C15 0.048(4) 0.065(5) 0.051(5) 0.009(4) -0.003(3) -0.004(3) C10A 0.052(4) 0.040(5) 0.045(4) 0.000(5) -0.005(3) -0.008(3) C11A 0.053(5) 0.064(7) 0.060(5) 0.001(5) -0.005(4) -0.016(5) C12A 0.051(5) 0.077(8) 0.073(6) -0.012(6) -0.003(5) -0.012(5) C13A 0.056(5) 0.080(7) 0.078(7) -0.010(7) -0.020(5) -0.018(5) C14A 0.065(6) 0.082(7) 0.066(6) -0.001(6) -0.023(5) -0.012(6) C15A 0.060(6) 0.073(7) 0.047(5) -0.001(5) -0.010(4) -0.018(5) C16 0.064(4) 0.046(3) 0.036(4) 0.007(3) -0.005(3) 0.001(3) C17 0.085(5) 0.059(4) 0.056(4) 0.005(4) 0.018(4) 0.012(4) C18 0.102(6) 0.072(5) 0.077(6) -0.006(4) 0.014(4) 0.027(4) C19 0.096(7) 0.066(5) 0.093(8) -0.012(6) 0.011(6) 0.028(5) C20 0.130(8) 0.062(5) 0.090(6) 0.001(5) 0.021(6) 0.031(5) C21 0.111(7) 0.042(4) 0.074(5) 0.004(4) 0.026(5) 0.007(4) C16A 0.059(4) 0.040(3) 0.050(4) 0.000(3) 0.004(4) -0.002(3) C17A 0.085(6) 0.050(4) 0.062(4) -0.021(4) -0.029(4) 0.011(4) C18A 0.087(6) 0.076(6) 0.090(6) -0.027(5) -0.019(5) 0.021(4) C19A 0.082(6) 0.058(5) 0.080(6) -0.015(5) 0.011(5) 0.010(4) C20A 0.086(6) 0.063(5) 0.058(4) -0.008(4) 0.014(4) 0.003(4) C21A 0.064(5) 0.065(5) 0.045(3) 0.005(3) 0.007(3) 0.003(3) P2 0.0339(4) 0.0438(5) 0.0367(4) 0.0028(4) -0.0021(3) 0.0029(4) C22 0.035(2) 0.049(4) 0.047(3) -0.009(3) -0.0050(18) 0.006(3) C23 0.047(3) 0.074(5) 0.051(3) -0.014(3) 0.004(3) -0.010(3) C24 0.048(3) 0.099(6) 0.069(4) -0.022(5) 0.003(3) -0.019(4) C25 0.040(3) 0.094(6) 0.094(5) -0.006(5) -0.011(3) 0.001(4) C26 0.058(3) 0.090(7) 0.077(4) 0.006(5) -0.033(3) -0.010(5) C27 0.053(3) 0.055(5) 0.054(3) 0.004(4) -0.013(3) -0.003(4) C22A 0.035(3) 0.052(6) 0.050(6) -0.008(5) -0.004(3) 0.009(4) C23A 0.049(4) 0.082(8) 0.061(7) -0.005(6) -0.003(5) -0.018(6) C24A 0.051(5) 0.095(8) 0.072(8) -0.009(6) -0.004(6) -0.015(6) C25A 0.054(6) 0.099(9) 0.080(8) -0.021(7) -0.015(5) -0.005(6) C26A 0.055(4) 0.069(8) 0.076(6) -0.009(6) -0.028(4) 0.013(6) C27A 0.046(4) 0.064(8) 0.059(5) -0.008(5) -0.012(4) 0.024(6) C28 0.041(4) 0.041(2) 0.058(4) 0.000(2) 0.002(3) 0.003(3) C29 0.116(6) 0.052(3) 0.060(4) 0.010(3) 0.009(5) 0.013(4) C30 0.124(7) 0.054(4) 0.082(5) 0.008(3) 0.017(5) 0.025(5) C31 0.081(6) 0.043(4) 0.094(6) 0.002(3) 0.017(5) 0.009(4) C32 0.073(5) 0.051(3) 0.088(5) -0.011(4) -0.001(5) 0.010(4) C33 0.067(5) 0.047(3) 0.070(4) -0.006(3) -0.016(4) 0.005(4) C28A 0.048(5) 0.043(3) 0.049(5) -0.005(3) -0.010(4) 0.005(3) C29A 0.117(8) 0.048(3) 0.067(6) -0.003(4) 0.020(5) -0.008(5) C30A 0.157(10) 0.050(4) 0.106(8) -0.002(5) 0.032(7) -0.003(6) C31A 0.108(9) 0.055(5) 0.107(8) -0.008(5) 0.005(6) 0.016(6) C32A 0.083(7) 0.061(4) 0.082(7) -0.018(5) -0.006(5) 0.017(6) C33A 0.061(6) 0.062(4) 0.077(6) -0.014(4) 0.011(5) 0.014(5) P3 0.0364(4) 0.0357(4) 0.0374(4) -0.0030(4) 0.0001(3) 0.0015(4) C34 0.029(2) 0.039(2) 0.041(3) -0.0031(19) 0.0100(19) -0.004(2) C35 0.067(4) 0.040(2) 0.055(3) -0.003(2) -0.007(3) -0.003(3) C36 0.083(5) 0.037(2) 0.075(4) 0.002(3) -0.006(3) -0.006(3) C37 0.063(4) 0.044(3) 0.060(4) -0.006(3) 0.014(3) -0.021(3) C38 0.095(6) 0.058(4) 0.042(3) -0.012(3) -0.008(3) -0.016(4) C39 0.083(5) 0.049(3) 0.040(3) 0.000(2) -0.006(3) -0.017(3) C34A 0.043(5) 0.049(4) 0.042(5) -0.004(3) 0.001(4) -0.009(4) C35A 0.063(7) 0.055(5) 0.055(5) 0.010(4) 0.004(5) -0.016(5) C36A 0.086(8) 0.058(6) 0.086(6) 0.013(5) 0.001(7) -0.022(6) C37A 0.073(8) 0.054(6) 0.101(7) -0.008(5) -0.003(7) -0.017(6) C38A 0.064(7) 0.054(6) 0.072(6) -0.022(5) -0.001(6) -0.003(6) C39A 0.047(7) 0.053(5) 0.048(5) -0.013(4) 0.001(5) -0.004(5) C40 0.036(3) 0.053(4) 0.053(4) -0.020(3) 0.002(3) 0.009(3) C41 0.059(5) 0.090(6) 0.115(7) 0.028(5) 0.026(5) 0.035(4) C42 0.055(5) 0.088(6) 0.114(7) -0.005(5) 0.007(4) 0.042(4) C43 0.048(5) 0.120(7) 0.069(6) -0.032(5) 0.008(4) 0.033(4) C44 0.071(6) 0.131(7) 0.091(7) 0.018(6) 0.040(5) 0.037(5) C45 0.070(5) 0.097(6) 0.081(6) 0.019(5) 0.037(4) 0.032(4) C40A 0.042(3) 0.062(5) 0.056(4) -0.003(3) 0.005(3) 0.012(3) C41A 0.048(3) 0.131(7) 0.074(5) -0.035(5) -0.002(4) 0.007(5) C42A 0.045(4) 0.160(8) 0.087(7) -0.028(6) -0.010(4) 0.029(5) C43A 0.057(4) 0.116(7) 0.085(6) -0.016(5) 0.009(5) 0.028(5) C44A 0.062(4) 0.096(7) 0.063(5) -0.013(4) 0.013(4) 0.013(5) C45A 0.048(4) 0.069(5) 0.055(4) -0.009(3) 0.006(3) 0.007(4) C7 0.051(2) 0.049(2) 0.0349(15) 0.0060(14) -0.0040(14) -0.0140(17) C8 0.0383(17) 0.0476(17) 0.0315(15) -0.0002(13) -0.0021(13) -0.0024(14) C9 0.0416(17) 0.0395(17) 0.0424(17) 0.0009(14) -0.0069(13) 0.0021(14) B1 0.0387(19) 0.0443(19) 0.0310(16) 0.0032(14) -0.0069(14) -0.0050(15) C1 0.053(2) 0.0504(19) 0.0343(16) 0.0051(14) -0.0086(15) -0.0090(17) C2 0.131(5) 0.059(3) 0.045(2) -0.0029(19) -0.030(3) 0.011(3) C3 0.137(5) 0.082(3) 0.040(2) -0.017(2) -0.031(3) 0.029(3) C4 0.098(4) 0.077(3) 0.047(2) 0.011(2) -0.018(3) -0.002(3) C5 0.104(4) 0.059(3) 0.057(2) 0.0073(19) -0.019(3) -0.001(3) C6 0.096(4) 0.059(2) 0.047(2) 0.0041(19) -0.012(2) 0.001(2) C1S 0.176(11) 0.084(7) 0.082(7) 0.002(5) -0.016(7) 0.024(7) C2S 0.185(11) 0.081(7) 0.083(7) 0.000(5) -0.004(7) 0.043(7) C3S 0.157(10) 0.090(8) 0.086(7) 0.023(5) -0.008(6) 0.023(7) C4S 0.189(11) 0.090(8) 0.073(7) 0.000(5) -0.003(7) -0.004(7) C5S 0.182(10) 0.053(6) 0.090(7) 0.009(5) 0.037(7) 0.009(6) C6S 0.149(9) 0.062(6) 0.112(8) 0.021(5) 0.010(7) 0.013(6) C1T 0.094(10) 0.090(10) 0.042(10) 0.016(10) -0.004(10) -0.018(8) C2T 0.097(9) 0.097(10) 0.018(9) 0.017(10) -0.004(9) -0.007(9) C3T 0.091(9) 0.094(11) 0.013(9) 0.015(9) 0.001(7) -0.017(8) C4T 0.092(10) 0.103(10) 0.020(9) 0.005(9) -0.006(9) -0.021(8) C5T 0.090(9) 0.093(10) 0.039(10) 0.026(10) 0.017(10) -0.024(9) C6T 0.102(9) 0.094(11) 0.045(10) 0.025(10) -0.002(10) -0.023(8) C1TA 0.094(10) 0.090(11) 0.021(8) 0.026(9) -0.003(9) -0.011(8) C2TA 0.095(9) 0.098(12) 0.007(11) 0.016(11) 0.002(9) -0.006(10) C3TA 0.092(10) 0.097(12) 0.018(10) 0.015(10) -0.003(9) -0.008(9) C4TA 0.097(11) 0.098(11) 0.025(10) 0.018(10) 0.001(10) -0.015(9) C5TA 0.092(10) 0.095(11) 0.026(10) 0.022(9) 0.008(10) -0.022(9) C6TA 0.093(10) 0.094(11) 0.036(10) 0.025(9) 0.009(9) -0.019(9) C1U 0.107(16) 0.093(16) 0.128(11) -0.012(10) 0.003(13) -0.013(12) C2U 0.095(13) 0.052(13) 0.140(13) -0.009(9) -0.004(13) -0.010(9) C3U 0.098(15) 0.034(11) 0.124(10) 0.009(8) -0.003(11) 0.024(11) C4U 0.085(14) 0.051(13) 0.112(10) -0.007(8) -0.020(11) 0.015(12) C5U 0.087(13) 0.062(14) 0.145(13) 0.002(10) -0.003(13) -0.005(10) C6U 0.109(16) 0.084(15) 0.119(10) 0.019(10) 0.000(13) -0.005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 Fe1 1.7525(15) . ? O1 Fe1 1.7525(15) 14_464 ? Fe1 P1 2.3953(11) . ? Fe1 P2 2.3969(10) . ? Fe1 P3 2.4096(10) . ? P1 C16 1.820(8) . ? P1 C7 1.824(4) . ? P1 C10 1.827(8) . ? P1 C10A 1.833(10) . ? P1 C16A 1.883(8) . ? C10 C11 1.374(9) . ? C10 C15 1.398(9) . ? C11 C12 1.391(10) . ? C12 C13 1.367(10) . ? C13 C14 1.353(10) . ? C14 C15 1.379(9) . ? C10A C11A 1.366(11) . ? C10A C15A 1.382(11) . ? C11A C12A 1.394(11) . ? C12A C13A 1.349(12) . ? C13A C14A 1.357(12) . ? C14A C15A 1.370(11) . ? C16 C21 1.366(10) . ? C16 C17 1.377(10) . ? C17 C18 1.383(10) . ? C18 C19 1.349(11) . ? C19 C20 1.363(11) . ? C20 C21 1.387(10) . ? C16A C17A 1.380(10) . ? C16A C21A 1.405(10) . ? C17A C18A 1.379(10) . ? C18A C19A 1.379(11) . ? C19A C20A 1.353(11) . ? C20A C21A 1.387(10) . ? P2 C8 1.815(4) . ? P2 C28A 1.817(9) . ? P2 C22A 1.833(10) . ? P2 C22 1.835(6) . ? P2 C28 1.856(7) . ? C22 C23 1.372(8) . ? C22 C27 1.386(8) . ? C23 C24 1.388(8) . ? C24 C25 1.355(10) . ? C25 C26 1.380(10) . ? C26 C27 1.382(8) . ? C22A C23A 1.376(12) . ? C22A C27A 1.387(12) . ? C23A C24A 1.390(12) . ? C24A C25A 1.366(12) . ? C25A C26A 1.348(12) . ? C26A C27A 1.383(12) . ? C28 C33 1.371(9) . ? C28 C29 1.388(9) . ? C29 C30 1.378(9) . ? C30 C31 1.342(10) . ? C31 C32 1.342(10) . ? C32 C33 1.381(9) . ? C28A C29A 1.369(11) . ? C28A C33A 1.373(10) . ? C29A C30A 1.383(11) . ? C30A C31A 1.353(12) . ? C31A C32A 1.340(12) . ? C32A C33A 1.397(11) . ? P3 C34A 1.811(10) . ? P3 C9 1.823(4) . ? P3 C40A 1.832(8) . ? P3 C34 1.835(6) . ? P3 C40 1.844(7) . ? C34 C35 1.386(8) . ? C34 C39 1.389(8) . ? C35 C36 1.391(8) . ? C36 C37 1.347(9) . ? C37 C38 1.367(9) . ? C38 C39 1.400(8) . ? C34A C35A 1.365(11) . ? C34A C39A 1.381(11) . ? C35A C36A 1.374(11) . ? C36A C37A 1.345(12) . ? C37A C38A 1.346(12) . ? C38A C39A 1.394(12) . ? C40 C41 1.370(10) . ? C40 C45 1.386(10) . ? C41 C42 1.398(10) . ? C42 C43 1.348(11) . ? C43 C44 1.357(11) . ? C44 C45 1.394(9) . ? C40A C41A 1.373(10) . ? C40A C45A 1.385(10) . ? C41A C42A 1.397(10) . ? C42A C43A 1.341(11) . ? C43A C44A 1.343(11) . ? C44A C45A 1.389(9) . ? C7 B1 1.651(5) . ? C8 B1 1.675(6) . ? C9 B1 1.678(6) . ? B1 C1 1.649(5) . ? C1 C2 1.364(6) . ? C1 C6 1.397(6) . ? C2 C3 1.381(7) . ? C3 C4 1.350(8) . ? C4 C5 1.381(7) . ? C5 C6 1.404(6) . ? C1S C6S 1.343(8) . ? C1S C2S 1.347(8) . ? C2S C3S 1.343(8) . ? C3S C4S 1.336(8) . ? C4S C5S 1.342(8) . ? C5S C6S 1.346(8) . ? C1T C6T 1.341(8) . ? C1T C2T 1.343(8) . ? C2T C3T 1.344(8) . ? C3T C4T 1.341(8) . ? C4T C5T 1.344(8) . ? C5T C6T 1.344(8) . ? C1TA C2TA 1.341(8) . ? C1TA C6TA 1.342(8) . ? C2TA C3TA 1.343(8) . ? C3TA C4TA 1.340(8) . ? C4TA C5TA 1.346(8) . ? C5TA C6TA 1.343(8) . ? C1U C2U 1.344(8) . ? C1U C6U 1.350(8) . ? C2U C3U 1.342(8) . ? C3U C4U 1.344(8) . ? C4U C5U 1.340(8) . ? C5U C6U 1.348(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 O1 Fe1 147.7(3) . 14_464 ? O1 Fe1 P1 120.54(9) . . ? O1 Fe1 P2 116.08(11) . . ? P1 Fe1 P2 88.96(4) . . ? O1 Fe1 P3 135.38(16) . . ? P1 Fe1 P3 92.94(4) . . ? P2 Fe1 P3 90.99(3) . . ? C16 P1 C7 104.1(3) . . ? C16 P1 C10 105.5(4) . . ? C7 P1 C10 105.5(4) . . ? C16 P1 C10A 102.6(4) . . ? C7 P1 C10A 109.3(5) . . ? C10 P1 C10A 4.1(7) . . ? C16 P1 C16A 7.4(5) . . ? C7 P1 C16A 111.0(3) . . ? C10 P1 C16A 100.6(4) . . ? C10A P1 C16A 97.5(4) . . ? C16 P1 Fe1 114.4(3) . . ? C7 P1 Fe1 111.34(13) . . ? C10 P1 Fe1 115.0(3) . . ? C10A P1 Fe1 114.3(4) . . ? C16A P1 Fe1 112.7(3) . . ? C11 C10 C15 117.6(8) . . ? C11 C10 P1 122.4(8) . . ? C15 C10 P1 120.0(7) . . ? C10 C11 C12 120.2(9) . . ? C13 C12 C11 120.5(9) . . ? C14 C13 C12 120.7(9) . . ? C13 C14 C15 119.2(8) . . ? C14 C15 C10 121.8(7) . . ? C11A C10A C15A 118.1(10) . . ? C11A C10A P1 123.7(11) . . ? C15A C10A P1 118.2(10) . . ? C10A C11A C12A 119.9(12) . . ? C13A C12A C11A 121.7(13) . . ? C12A C13A C14A 118.1(13) . . ? C13A C14A C15A 121.6(12) . . ? C14A C15A C10A 120.5(10) . . ? C21 C16 C17 119.2(8) . . ? C21 C16 P1 122.7(7) . . ? C17 C16 P1 118.2(7) . . ? C16 C17 C18 119.7(8) . . ? C19 C18 C17 121.4(10) . . ? C18 C19 C20 118.7(10) . . ? C19 C20 C21 121.2(10) . . ? C16 C21 C20 119.7(9) . . ? C17A C16A C21A 117.6(8) . . ? C17A C16A P1 123.0(7) . . ? C21A C16A P1 119.3(7) . . ? C18A C17A C16A 119.4(8) . . ? C19A C18A C17A 121.6(10) . . ? C20A C19A C18A 119.3(10) . . ? C19A C20A C21A 119.8(9) . . ? C20A C21A C16A 121.3(8) . . ? C8 P2 C28A 111.1(3) . . ? C8 P2 C22A 110.3(5) . . ? C28A P2 C22A 102.0(5) . . ? C8 P2 C22 106.6(3) . . ? C28A P2 C22 103.8(4) . . ? C22A P2 C22 3.7(7) . . ? C8 P2 C28 105.2(3) . . ? C28A P2 C28 11.3(5) . . ? C22A P2 C28 95.6(4) . . ? C22 P2 C28 96.9(3) . . ? C8 P2 Fe1 110.48(12) . . ? C28A P2 Fe1 114.4(4) . . ? C22A P2 Fe1 108.3(4) . . ? C22 P2 Fe1 110.1(2) . . ? C28 P2 Fe1 125.6(2) . . ? C23 C22 C27 119.8(6) . . ? C23 C22 P2 123.0(6) . . ? C27 C22 P2 117.2(6) . . ? C22 C23 C24 120.1(7) . . ? C25 C24 C23 120.5(8) . . ? C24 C25 C26 119.6(8) . . ? C25 C26 C27 120.7(7) . . ? C26 C27 C22 119.2(7) . . ? C23A C22A C27A 116.4(11) . . ? C23A C22A P2 125.9(11) . . ? C27A C22A P2 117.7(10) . . ? C22A C23A C24A 120.0(12) . . ? C25A C24A C23A 123.5(13) . . ? C26A C25A C24A 116.0(13) . . ? C25A C26A C27A 122.3(13) . . ? C26A C27A C22A 121.6(12) . . ? C33 C28 C29 116.0(7) . . ? C33 C28 P2 125.9(6) . . ? C29 C28 P2 118.0(6) . . ? C30 C29 C28 121.8(8) . . ? C31 C30 C29 120.8(9) . . ? C32 C31 C30 117.9(8) . . ? C31 C32 C33 122.8(9) . . ? C28 C33 C32 120.4(8) . . ? C29A C28A C33A 119.3(9) . . ? C29A C28A P2 122.0(8) . . ? C33A C28A P2 118.7(8) . . ? C28A C29A C30A 119.9(10) . . ? C31A C30A C29A 120.8(11) . . ? C32A C31A C30A 119.5(11) . . ? C31A C32A C33A 121.4(11) . . ? C28A C33A C32A 118.8(10) . . ? C34A P3 C9 115.2(4) . . ? C34A P3 C40A 102.6(4) . . ? C9 P3 C40A 105.7(3) . . ? C34A P3 C34 11.0(5) . . ? C9 P3 C34 104.8(2) . . ? C40A P3 C34 110.2(3) . . ? C34A P3 C40 92.5(4) . . ? C9 P3 C40 105.4(3) . . ? C40A P3 C40 11.7(4) . . ? C34 P3 C40 99.4(3) . . ? C34A P3 Fe1 110.3(3) . . ? C9 P3 Fe1 107.34(12) . . ? C40A P3 Fe1 115.9(3) . . ? C34 P3 Fe1 112.12(19) . . ? C40 P3 Fe1 125.9(2) . . ? C35 C34 C39 117.3(5) . . ? C35 C34 P3 119.0(5) . . ? C39 C34 P3 123.7(5) . . ? C34 C35 C36 122.0(6) . . ? C37 C36 C35 120.0(6) . . ? C36 C37 C38 119.6(6) . . ? C37 C38 C39 121.2(6) . . ? C34 C39 C38 119.8(6) . . ? C35A C34A C39A 121.4(10) . . ? C35A C34A P3 118.5(9) . . ? C39A C34A P3 120.1(9) . . ? C34A C35A C36A 117.7(11) . . ? C37A C36A C35A 121.8(12) . . ? C36A C37A C38A 120.8(12) . . ? C37A C38A C39A 119.5(12) . . ? C34A C39A C38A 118.5(11) . . ? C41 C40 C45 116.7(8) . . ? C41 C40 P3 123.3(7) . . ? C45 C40 P3 119.6(6) . . ? C40 C41 C42 120.3(9) . . ? C43 C42 C41 122.9(9) . . ? C42 C43 C44 116.0(9) . . ? C43 C44 C45 122.6(10) . . ? C40 C45 C44 120.0(9) . . ? C41A C40A C45A 116.4(8) . . ? C41A C40A P3 123.2(7) . . ? C45A C40A P3 120.4(7) . . ? C40A C41A C42A 120.8(9) . . ? C43A C42A C41A 119.8(10) . . ? C42A C43A C44A 120.7(9) . . ? C43A C44A C45A 118.7(9) . . ? C40A C45A C44A 122.1(8) . . ? B1 C7 P1 116.2(3) . . ? B1 C8 P2 116.7(2) . . ? B1 C9 P3 119.0(3) . . ? C1 B1 C7 109.7(3) . . ? C1 B1 C8 110.3(3) . . ? C7 B1 C8 110.6(3) . . ? C1 B1 C9 103.3(3) . . ? C7 B1 C9 111.2(3) . . ? C8 B1 C9 111.4(3) . . ? C2 C1 C6 114.7(4) . . ? C2 C1 B1 123.9(4) . . ? C6 C1 B1 121.0(4) . . ? C1 C2 C3 123.3(5) . . ? C4 C3 C2 121.2(5) . . ? C3 C4 C5 118.6(5) . . ? C4 C5 C6 118.9(5) . . ? C1 C6 C5 122.9(5) . . ? C6S C1S C2S 120.6(8) . . ? C3S C2S C1S 120.2(8) . . ? C4S C3S C2S 119.2(8) . . ? C3S C4S C5S 120.9(8) . . ? C4S C5S C6S 120.3(8) . . ? C1S C6S C5S 118.9(8) . . ? C6T C1T C2T 119.7(9) . . ? C1T C2T C3T 120.0(9) . . ? C4T C3T C2T 120.4(9) . . ? C3T C4T C5T 119.7(9) . . ? C6T C5T C4T 119.9(9) . . ? C1T C6T C5T 120.4(9) . . ? C2TA C1TA C6TA 120.2(9) . . ? C1TA C2TA C3TA 119.6(9) . . ? C4TA C3TA C2TA 120.4(9) . . ? C3TA C4TA C5TA 120.0(9) . . ? C6TA C5TA C4TA 119.7(9) . . ? C1TA C6TA C5TA 120.1(9) . . ? C2U C1U C6U 120.2(9) . . ? C3U C2U C1U 119.6(8) . . ? C2U C3U C4U 120.3(9) . . ? C5U C4U C3U 120.3(9) . . ? C4U C5U C6U 119.7(8) . . ? C5U C6U C1U 119.9(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.61 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.761 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 937863' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H81 B1 Fe1 Na1 O7 P3' _chemical_formula_weight 1180.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M p3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 13.1184(19) _cell_length_b 13.1184(19) _cell_length_c 31.059(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4628.9(13) _cell_formula_units_Z 3 _cell_measurement_temperature 77 _cell_measurement_reflns_used 38888 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 28.43 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1878 _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystals grown from a THF/petroleum ether layer at -35 oC ; _diffrn_ambient_temperature 77(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 3 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38888 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.43 _reflns_number_total 13916 _reflns_number_gt 12610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some of the THFs that coordinate the Na appear to be disordered; however modelling the disorder did not lead to an improvement of the model (and several atoms went NPD), so the disorder was not modelled. The dataset is 99.9 % complete to theta = 27.0. The missing high angle data may be due to the square detector employed. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(11) _refine_ls_number_reflns 13916 _refine_ls_number_parameters 741 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40964(3) 0.30295(3) 0.256633(11) 0.01222(8) Uani 1 1 d . . . P1 P 0.29681(5) 0.38193(6) 0.26743(2) 0.01230(13) Uani 1 1 d . . . P2 P 0.27673(6) 0.12685(6) 0.28035(2) 0.01282(13) Uani 1 1 d . . . P3 P 0.32617(6) 0.25001(6) 0.19053(2) 0.01213(13) Uani 1 1 d . . . Na1 Na 0.77391(10) 0.55896(10) 0.34765(4) 0.0230(2) Uani 1 1 d . . . O1 O 0.6348(2) 0.3470(2) 0.22240(8) 0.0381(6) Uani 1 1 d . . . O2 O 0.56337(18) 0.4180(2) 0.32962(7) 0.0260(5) Uani 1 1 d . . . O3 O 0.8047(2) 0.3970(2) 0.35196(10) 0.0431(6) Uani 1 1 d . . . O4 O 0.7251(3) 0.5548(2) 0.42017(9) 0.0578(9) Uani 1 1 d . B . O5 O 0.73873(19) 0.71565(19) 0.33956(8) 0.0319(5) Uani 1 1 d . . . O6 O 0.8403(2) 0.6015(3) 0.27493(8) 0.0454(7) Uani 1 1 d . . . O7 O 0.9674(2) 0.6794(2) 0.37440(8) 0.0339(5) Uani 1 1 d . . . C1 C -0.0401(2) 0.0942(2) 0.22361(9) 0.0183(5) Uani 1 1 d . . . C2 C -0.0934(3) -0.0122(3) 0.20124(14) 0.0400(9) Uani 1 1 d . . . H2 H -0.0470 -0.0443 0.1933 0.048 Uiso 1 1 calc R . . C3 C -0.2108(3) -0.0725(3) 0.19027(14) 0.0447(10) Uani 1 1 d . . . H3 H -0.2414 -0.1430 0.1752 0.054 Uiso 1 1 calc R . . C4 C -0.2833(3) -0.0286(3) 0.20152(12) 0.0320(7) Uani 1 1 d . . . H4 H -0.3633 -0.0699 0.1951 0.038 Uiso 1 1 calc R . . C5 C -0.2339(3) 0.0779(4) 0.22254(14) 0.0428(9) Uani 1 1 d . . . H5 H -0.2801 0.1109 0.2295 0.051 Uiso 1 1 calc R . . C6 C -0.1153(3) 0.1364(3) 0.23338(12) 0.0362(8) Uani 1 1 d . . . H6 H -0.0847 0.2076 0.2480 0.043 Uiso 1 1 calc R . . C7 C 0.1392(2) 0.2749(2) 0.26720(8) 0.0145(5) Uani 1 1 d . . . H7A H 0.1151 0.2450 0.2962 0.017 Uiso 1 1 calc R . . H7B H 0.0966 0.3146 0.2589 0.017 Uiso 1 1 calc R . . C8 C 0.1350(2) 0.0621(2) 0.25274(9) 0.0165(5) Uani 1 1 d . . . H8A H 0.1359 0.0150 0.2288 0.020 Uiso 1 1 calc R . . H8B H 0.0738 0.0098 0.2725 0.020 Uiso 1 1 calc R . . C9 C 0.1732(2) 0.2158(2) 0.18820(8) 0.0151(5) Uani 1 1 d . . . H9A H 0.1714 0.2868 0.1811 0.018 Uiso 1 1 calc R . . H9B H 0.1331 0.1591 0.1654 0.018 Uiso 1 1 calc R . . C10 C 0.3215(2) 0.4980(2) 0.22832(8) 0.0155(5) Uani 1 1 d . . . C11 C 0.4382(2) 0.5698(2) 0.21487(9) 0.0193(5) Uani 1 1 d . . . H11 H 0.4961 0.5546 0.2248 0.023 Uiso 1 1 calc R . . C12 C 0.4685(3) 0.6630(3) 0.18698(10) 0.0249(6) Uani 1 1 d . . . H12 H 0.5465 0.7107 0.1787 0.030 Uiso 1 1 calc R . . C13 C 0.3822(3) 0.6850(3) 0.17151(9) 0.0252(6) Uani 1 1 d . . . H13 H 0.4024 0.7482 0.1531 0.030 Uiso 1 1 calc R . . C14 C 0.2664(3) 0.6133(3) 0.18342(9) 0.0233(6) Uani 1 1 d . . . H14 H 0.2083 0.6266 0.1723 0.028 Uiso 1 1 calc R . . C15 C 0.2363(2) 0.5210(2) 0.21213(9) 0.0192(5) Uani 1 1 d . . . H15 H 0.1582 0.4742 0.2206 0.023 Uiso 1 1 calc R . . C16 C 0.3139(2) 0.4640(2) 0.31791(8) 0.0143(5) Uani 1 1 d . . . C17 C 0.3258(2) 0.4180(2) 0.35691(9) 0.0190(5) Uani 1 1 d . . . H17 H 0.3242 0.3463 0.3572 0.023 Uiso 1 1 calc R . . C18 C 0.3400(3) 0.4781(3) 0.39535(9) 0.0217(6) Uani 1 1 d . . . H18 H 0.3483 0.4466 0.4210 0.026 Uiso 1 1 calc R . . C19 C 0.3417(3) 0.5844(3) 0.39564(9) 0.0230(6) Uani 1 1 d . . . H19 H 0.3529 0.6253 0.4213 0.028 Uiso 1 1 calc R . . C20 C 0.3266(3) 0.6292(3) 0.35732(10) 0.0243(6) Uani 1 1 d . . . H20 H 0.3257 0.6996 0.3573 0.029 Uiso 1 1 calc R . . C21 C 0.3129(2) 0.5692(2) 0.31887(9) 0.0192(5) Uani 1 1 d . . . H21 H 0.3029 0.6002 0.2933 0.023 Uiso 1 1 calc R . . C22 C 0.2356(2) 0.1159(2) 0.33775(8) 0.0146(5) Uani 1 1 d . . . C23 C 0.3212(3) 0.1446(2) 0.36939(9) 0.0192(5) Uani 1 1 d . . . H23 H 0.3981 0.1682 0.3612 0.023 Uiso 1 1 calc R . . C24 C 0.2939(3) 0.1388(3) 0.41277(10) 0.0252(6) Uani 1 1 d . . . H24 H 0.3520 0.1575 0.4334 0.030 Uiso 1 1 calc R . . C25 C 0.1794(3) 0.1048(3) 0.42550(10) 0.0280(7) Uani 1 1 d . . . H25 H 0.1610 0.1013 0.4546 0.034 Uiso 1 1 calc R . . C26 C 0.0939(3) 0.0764(3) 0.39478(10) 0.0245(6) Uani 1 1 d . . . H26 H 0.0172 0.0529 0.4032 0.029 Uiso 1 1 calc R . . C27 C 0.1212(3) 0.0825(2) 0.35107(9) 0.0205(6) Uani 1 1 d . . . H27 H 0.0627 0.0642 0.3306 0.025 Uiso 1 1 calc R . . C28 C 0.3219(2) 0.0142(2) 0.27869(8) 0.0160(5) Uani 1 1 d . . . C29 C 0.4385(3) 0.0477(3) 0.28752(9) 0.0218(6) Uani 1 1 d . . . H29 H 0.4906 0.1251 0.2955 0.026 Uiso 1 1 calc R . . C30 C 0.4787(3) -0.0317(3) 0.28466(10) 0.0262(6) Uani 1 1 d . . . H30 H 0.5565 -0.0080 0.2914 0.031 Uiso 1 1 calc R . . C31 C 0.4021(3) -0.1471(3) 0.27172(10) 0.0268(6) Uani 1 1 d . . . H31 H 0.4288 -0.2004 0.2691 0.032 Uiso 1 1 calc R . . C32 C 0.2864(3) -0.1815(3) 0.26280(10) 0.0261(6) Uani 1 1 d . . . H32 H 0.2350 -0.2585 0.2542 0.031 Uiso 1 1 calc R . . C33 C 0.2456(3) -0.1021(2) 0.26657(9) 0.0212(6) Uani 1 1 d . . . H33 H 0.1670 -0.1269 0.2610 0.025 Uiso 1 1 calc R . . C34 C 0.3238(2) 0.1185(2) 0.16736(8) 0.0148(5) Uani 1 1 d . . . C35 C 0.4065(3) 0.0878(2) 0.18012(9) 0.0198(6) Uani 1 1 d . . . H35 H 0.4612 0.1320 0.2013 0.024 Uiso 1 1 calc R . . C36 C 0.4092(3) -0.0080(3) 0.16182(10) 0.0252(6) Uani 1 1 d . . . H36 H 0.4652 -0.0271 0.1707 0.030 Uiso 1 1 calc R . . C37 C 0.3287(3) -0.0742(3) 0.13053(11) 0.0270(6) Uani 1 1 d . . . H37 H 0.3303 -0.1381 0.1183 0.032 Uiso 1 1 calc R . . C38 C 0.2456(3) -0.0455(3) 0.11744(11) 0.0305(7) Uani 1 1 d . . . H38 H 0.1906 -0.0907 0.0966 0.037 Uiso 1 1 calc R . . C39 C 0.2441(3) 0.0506(3) 0.13538(10) 0.0262(6) Uani 1 1 d . . . H39 H 0.1887 0.0700 0.1259 0.031 Uiso 1 1 calc R . . C40 C 0.3993(2) 0.3499(2) 0.14457(8) 0.0160(5) Uani 1 1 d . . . C41 C 0.3511(3) 0.4073(3) 0.12292(10) 0.0267(6) Uani 1 1 d . . . H41 H 0.2784 0.3966 0.1315 0.032 Uiso 1 1 calc R . . C42 C 0.4098(3) 0.4816(3) 0.08822(10) 0.0315(7) Uani 1 1 d . . . H42 H 0.3758 0.5194 0.0739 0.038 Uiso 1 1 calc R . . C43 C 0.5168(3) 0.4989(3) 0.07524(10) 0.0319(7) Uani 1 1 d . . . H43 H 0.5560 0.5492 0.0524 0.038 Uiso 1 1 calc R . . C44 C 0.5666(3) 0.4418(3) 0.09609(11) 0.0320(7) Uani 1 1 d . . . H44 H 0.6389 0.4525 0.0870 0.038 Uiso 1 1 calc R . . C45 C 0.5091(3) 0.3681(3) 0.13081(10) 0.0257(6) Uani 1 1 d . . . H45 H 0.5437 0.3306 0.1450 0.031 Uiso 1 1 calc R . . C46 C 0.5435(2) 0.3291(3) 0.23450(9) 0.0220(6) Uani 1 1 d . . . C47 C 0.4977(2) 0.3710(2) 0.30174(9) 0.0191(6) Uani 1 1 d . . . C48 C 0.9022(4) 0.3942(4) 0.37086(17) 0.0571(12) Uani 1 1 d . . . H48A H 0.8887 0.3761 0.4013 0.068 Uiso 1 1 calc R . . H48B H 0.9737 0.4696 0.3674 0.068 Uiso 1 1 calc R . . C49 C 0.9117(4) 0.3001(4) 0.34754(16) 0.0562(12) Uani 1 1 d . . . H49A H 0.9500 0.2678 0.3651 0.067 Uiso 1 1 calc R . . H49B H 0.9544 0.3290 0.3207 0.067 Uiso 1 1 calc R . . C50 C 0.7832(4) 0.2097(4) 0.33964(15) 0.0498(10) Uani 1 1 d . . . H50A H 0.7744 0.1608 0.3149 0.060 Uiso 1 1 calc R . . H50B H 0.7482 0.1599 0.3646 0.060 Uiso 1 1 calc R . . C51 C 0.7298(4) 0.2853(4) 0.33144(15) 0.0476(10) Uani 1 1 d . . . H51A H 0.7252 0.2960 0.3007 0.057 Uiso 1 1 calc R . . H51B H 0.6510 0.2490 0.3434 0.057 Uiso 1 1 calc R . . C52 C 0.6937(7) 0.4561(5) 0.44695(19) 0.087(2) Uani 1 1 d . . . H52A H 0.7527 0.4322 0.4463 0.105 Uiso 1 1 calc R A 1 H52B H 0.6178 0.3899 0.4391 0.105 Uiso 1 1 calc R A 1 C53A C 0.6897(17) 0.5048(14) 0.4885(4) 0.077(6) Uani 0.438(15) 1 d P B 1 H53A H 0.7675 0.5447 0.5013 0.093 Uiso 0.438(15) 1 calc PR B 1 H53B H 0.6371 0.4422 0.5077 0.093 Uiso 0.438(15) 1 calc PR B 1 C53B C 0.5962(8) 0.4289(9) 0.4697(3) 0.053(3) Uani 0.562(15) 1 d P B 2 H53C H 0.5920 0.3861 0.4957 0.063 Uiso 0.562(15) 1 calc PR B 2 H53D H 0.5257 0.3824 0.4527 0.063 Uiso 0.562(15) 1 calc PR B 2 C54A C 0.646(3) 0.592(4) 0.4819(7) 0.087(7) Uani 0.63(6) 1 d P B 1 H54A H 0.5608 0.5528 0.4794 0.105 Uiso 0.63(6) 1 calc PR B 1 H54B H 0.6730 0.6513 0.5042 0.105 Uiso 0.63(6) 1 calc PR B 1 C54B C 0.6113(16) 0.542(3) 0.4794(7) 0.043(7) Uani 0.37(6) 1 d P B 2 H54C H 0.6434 0.5656 0.5081 0.051 Uiso 0.37(6) 1 calc PR B 2 H54D H 0.5362 0.5390 0.4782 0.051 Uiso 0.37(6) 1 calc PR B 2 C55 C 0.7001(6) 0.6335(5) 0.44448(17) 0.0717(15) Uani 1 1 d . . . H55A H 0.7737 0.7054 0.4500 0.086 Uiso 1 1 calc R B 1 H55B H 0.6518 0.6538 0.4269 0.086 Uiso 1 1 calc R B 1 C56 C 0.8311(3) 0.8349(3) 0.34277(15) 0.0421(9) Uani 1 1 d . . . H56A H 0.8809 0.8570 0.3174 0.051 Uiso 1 1 calc R . . H56B H 0.8792 0.8454 0.3679 0.051 Uiso 1 1 calc R . . C57 C 0.7751(4) 0.9083(4) 0.3464(2) 0.0737(17) Uani 1 1 d . . . H57A H 0.8220 0.9834 0.3320 0.088 Uiso 1 1 calc R . . H57B H 0.7650 0.9224 0.3763 0.088 Uiso 1 1 calc R . . C58 C 0.6596(4) 0.8378(5) 0.3248(2) 0.0666(14) Uani 1 1 d . . . H58A H 0.6006 0.8514 0.3381 0.080 Uiso 1 1 calc R . . H58B H 0.6652 0.8578 0.2945 0.080 Uiso 1 1 calc R . . C59 C 0.6295(3) 0.7137(4) 0.33044(16) 0.0458(10) Uani 1 1 d . . . H59A H 0.5745 0.6778 0.3541 0.055 Uiso 1 1 calc R . . H59B H 0.5937 0.6691 0.3044 0.055 Uiso 1 1 calc R . . C60 C 0.9106(4) 0.5669(6) 0.25005(16) 0.0780(19) Uani 1 1 d . . . H60A H 0.8667 0.4840 0.2428 0.094 Uiso 1 1 calc R . . H60B H 0.9818 0.5834 0.2653 0.094 Uiso 1 1 calc R . . C61 C 0.9390(6) 0.6451(6) 0.20942(19) 0.118(3) Uani 1 1 d . . . H61A H 1.0020 0.7248 0.2149 0.142 Uiso 1 1 calc R . . H61B H 0.9605 0.6126 0.1853 0.142 Uiso 1 1 calc R . . C62 C 0.8240(6) 0.6412(5) 0.20144(15) 0.0794(19) Uani 1 1 d . . . H62A H 0.7689 0.5699 0.1864 0.095 Uiso 1 1 calc R . . H62B H 0.8355 0.7090 0.1849 0.095 Uiso 1 1 calc R . . C63 C 0.7816(5) 0.6435(4) 0.24649(13) 0.0589(12) Uani 1 1 d . . . H63A H 0.8014 0.7229 0.2543 0.071 Uiso 1 1 calc R . . H63B H 0.6969 0.5929 0.2484 0.071 Uiso 1 1 calc R . . C64 C 1.0675(3) 0.7443(3) 0.34698(11) 0.0395(8) Uani 1 1 d . . . H64A H 1.0535 0.7931 0.3272 0.047 Uiso 1 1 calc R . . H64B H 1.0832 0.6909 0.3304 0.047 Uiso 1 1 calc R . . C65 C 1.1701(3) 0.8197(3) 0.37598(12) 0.0336(7) Uani 1 1 d . . . H65A H 1.1759 0.8951 0.3816 0.040 Uiso 1 1 calc R . . H65B H 1.2437 0.8324 0.3639 0.040 Uiso 1 1 calc R . . C66 C 1.1375(3) 0.7449(4) 0.41605(12) 0.0417(9) Uani 1 1 d . . . H66A H 1.1568 0.6828 0.4132 0.050 Uiso 1 1 calc R . . H66B H 1.1768 0.7920 0.4412 0.050 Uiso 1 1 calc R . . C67 C 1.0066(3) 0.6954(4) 0.41852(12) 0.0422(9) Uani 1 1 d . . . H67A H 0.9691 0.6209 0.4338 0.051 Uiso 1 1 calc R . . H67B H 0.9884 0.7496 0.4332 0.051 Uiso 1 1 calc R . . B1 B 0.1017(3) 0.1618(3) 0.23412(9) 0.0154(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01124(17) 0.01267(17) 0.01187(17) -0.00129(14) -0.00104(14) 0.00532(14) P1 0.0121(3) 0.0119(3) 0.0122(3) -0.0006(2) -0.0006(2) 0.0054(3) P2 0.0135(3) 0.0123(3) 0.0118(3) -0.0008(2) -0.0012(2) 0.0059(3) P3 0.0117(3) 0.0127(3) 0.0119(3) -0.0006(2) -0.0002(2) 0.0061(3) Na1 0.0228(6) 0.0237(6) 0.0206(6) -0.0024(4) -0.0021(4) 0.0102(5) O1 0.0186(11) 0.0575(16) 0.0324(13) -0.0150(11) 0.0000(9) 0.0148(11) O2 0.0204(10) 0.0348(12) 0.0203(11) -0.0101(9) -0.0081(8) 0.0120(9) O3 0.0393(14) 0.0381(14) 0.0597(17) -0.0189(12) -0.0232(13) 0.0252(12) O4 0.095(2) 0.0384(15) 0.0353(15) 0.0064(12) 0.0277(15) 0.0301(16) O5 0.0188(11) 0.0235(11) 0.0514(15) 0.0011(10) -0.0016(10) 0.0090(9) O6 0.0337(13) 0.075(2) 0.0228(12) -0.0095(12) -0.0006(10) 0.0241(14) O7 0.0273(12) 0.0371(13) 0.0241(11) 0.0013(10) -0.0076(9) 0.0062(10) C1 0.0152(12) 0.0193(13) 0.0166(13) 0.0005(10) -0.0009(10) 0.0058(11) C2 0.0209(16) 0.0348(19) 0.065(3) -0.0210(17) -0.0139(16) 0.0146(14) C3 0.0307(18) 0.0324(19) 0.069(3) -0.0260(18) -0.0243(18) 0.0144(16) C4 0.0121(13) 0.0344(18) 0.0392(19) -0.0044(14) -0.0050(12) 0.0038(13) C5 0.0192(16) 0.051(2) 0.059(3) -0.0243(19) -0.0065(16) 0.0176(16) C6 0.0208(16) 0.0339(18) 0.049(2) -0.0207(15) -0.0080(14) 0.0101(14) C7 0.0122(12) 0.0130(12) 0.0185(13) -0.0013(10) 0.0006(9) 0.0063(10) C8 0.0150(12) 0.0153(12) 0.0153(13) -0.0012(10) -0.0011(10) 0.0045(10) C9 0.0147(12) 0.0169(12) 0.0146(13) -0.0019(10) -0.0026(10) 0.0086(11) C10 0.0207(13) 0.0125(12) 0.0136(12) -0.0020(9) -0.0013(10) 0.0085(10) C11 0.0200(14) 0.0182(13) 0.0187(13) -0.0008(10) -0.0017(11) 0.0088(11) C12 0.0239(15) 0.0194(14) 0.0257(16) 0.0020(11) -0.0002(12) 0.0067(12) C13 0.0383(17) 0.0184(14) 0.0171(14) 0.0029(11) -0.0004(12) 0.0129(13) C14 0.0318(16) 0.0286(15) 0.0168(13) -0.0024(11) -0.0058(12) 0.0204(14) C15 0.0183(13) 0.0230(14) 0.0166(13) -0.0017(11) -0.0008(10) 0.0106(11) C16 0.0103(11) 0.0146(12) 0.0152(12) -0.0037(9) -0.0008(9) 0.0041(10) C17 0.0227(14) 0.0153(13) 0.0177(13) -0.0006(10) 0.0026(11) 0.0086(11) C18 0.0279(15) 0.0218(14) 0.0126(13) 0.0005(10) 0.0019(11) 0.0103(12) C19 0.0266(15) 0.0224(14) 0.0168(14) -0.0043(11) 0.0034(11) 0.0098(12) C20 0.0302(16) 0.0205(14) 0.0257(16) -0.0048(12) -0.0005(12) 0.0154(13) C21 0.0242(14) 0.0185(13) 0.0165(13) -0.0015(10) -0.0025(10) 0.0118(12) C22 0.0217(13) 0.0097(11) 0.0124(12) 0.0014(9) 0.0014(10) 0.0079(10) C23 0.0224(14) 0.0166(13) 0.0192(14) -0.0013(10) -0.0010(11) 0.0101(11) C24 0.0333(16) 0.0274(15) 0.0160(14) -0.0015(11) -0.0045(12) 0.0160(13) C25 0.0395(18) 0.0293(16) 0.0150(14) 0.0008(11) 0.0056(12) 0.0170(14) C26 0.0267(15) 0.0231(14) 0.0232(15) -0.0007(12) 0.0071(12) 0.0121(12) C27 0.0241(14) 0.0182(13) 0.0191(14) -0.0031(10) 0.0004(11) 0.0106(12) C28 0.0213(13) 0.0148(12) 0.0137(12) 0.0009(9) 0.0026(10) 0.0103(11) C29 0.0230(14) 0.0195(14) 0.0222(14) -0.0007(11) -0.0024(11) 0.0101(12) C30 0.0254(15) 0.0327(16) 0.0276(16) 0.0026(13) -0.0008(12) 0.0200(14) C31 0.0394(18) 0.0232(15) 0.0268(16) 0.0056(12) 0.0075(13) 0.0225(14) C32 0.0318(16) 0.0164(14) 0.0278(16) -0.0028(11) 0.0015(12) 0.0104(13) C33 0.0230(14) 0.0207(14) 0.0197(14) -0.0012(11) -0.0007(11) 0.0108(12) C34 0.0175(12) 0.0129(12) 0.0133(12) -0.0003(9) 0.0022(10) 0.0070(10) C35 0.0210(14) 0.0211(14) 0.0184(14) -0.0011(11) 0.0000(11) 0.0115(12) C36 0.0291(16) 0.0290(16) 0.0253(15) -0.0021(12) 0.0019(12) 0.0203(13) C37 0.0327(16) 0.0231(15) 0.0287(16) -0.0029(12) 0.0023(13) 0.0166(13) C38 0.0290(16) 0.0291(16) 0.0357(18) -0.0168(14) -0.0116(14) 0.0162(14) C39 0.0266(15) 0.0301(16) 0.0286(16) -0.0091(13) -0.0078(12) 0.0193(13) C40 0.0206(13) 0.0140(12) 0.0112(12) -0.0005(9) 0.0013(10) 0.0069(11) C41 0.0303(16) 0.0315(16) 0.0244(16) 0.0067(12) 0.0076(12) 0.0201(14) C42 0.048(2) 0.0361(18) 0.0241(16) 0.0138(13) 0.0090(14) 0.0309(16) C43 0.0423(19) 0.0279(16) 0.0211(15) 0.0085(12) 0.0112(13) 0.0144(15) C44 0.0297(17) 0.0345(18) 0.0322(18) 0.0112(14) 0.0129(13) 0.0162(14) C45 0.0226(15) 0.0299(16) 0.0247(15) 0.0090(12) 0.0039(12) 0.0133(13) C46 0.0159(13) 0.0304(15) 0.0177(14) -0.0082(11) -0.0030(10) 0.0100(12) C47 0.0159(13) 0.0191(13) 0.0227(14) -0.0018(11) 0.0017(11) 0.0090(11) C48 0.058(3) 0.065(3) 0.066(3) -0.026(2) -0.027(2) 0.044(2) C49 0.060(3) 0.073(3) 0.058(3) -0.024(2) -0.015(2) 0.050(3) C50 0.057(3) 0.040(2) 0.056(3) -0.0023(19) 0.004(2) 0.027(2) C51 0.053(2) 0.043(2) 0.047(2) -0.0145(18) -0.0162(19) 0.024(2) C52 0.142(6) 0.045(3) 0.063(3) 0.026(2) 0.042(4) 0.038(3) C53A 0.131(15) 0.084(10) 0.036(6) 0.022(6) 0.017(7) 0.068(11) C53B 0.047(5) 0.073(6) 0.047(5) 0.037(4) 0.024(4) 0.036(5) C54A 0.137(17) 0.113(17) 0.062(8) 0.037(9) 0.044(10) 0.100(15) C54B 0.029(9) 0.082(16) 0.028(7) 0.005(9) 0.010(5) 0.036(9) C55 0.100(4) 0.065(3) 0.051(3) -0.009(2) 0.025(3) 0.042(3) C56 0.0288(18) 0.0269(17) 0.067(3) 0.0012(17) -0.0005(17) 0.0112(15) C57 0.044(3) 0.035(2) 0.144(6) -0.001(3) -0.006(3) 0.021(2) C58 0.053(3) 0.063(3) 0.097(4) 0.015(3) -0.002(3) 0.039(2) C59 0.0241(17) 0.043(2) 0.070(3) 0.0070(19) -0.0011(17) 0.0164(16) C60 0.032(2) 0.133(5) 0.051(3) -0.054(3) -0.011(2) 0.028(3) C61 0.067(4) 0.112(5) 0.062(4) -0.043(3) 0.036(3) -0.041(4) C62 0.117(5) 0.054(3) 0.027(2) 0.007(2) 0.007(3) 0.013(3) C63 0.082(3) 0.052(3) 0.028(2) 0.0069(18) -0.006(2) 0.023(2) C64 0.0298(17) 0.047(2) 0.0277(18) 0.0050(15) -0.0037(14) 0.0090(16) C65 0.0306(17) 0.0232(15) 0.047(2) -0.0074(14) -0.0123(15) 0.0133(14) C66 0.043(2) 0.061(3) 0.0306(18) -0.0091(17) -0.0179(16) 0.033(2) C67 0.046(2) 0.058(2) 0.0224(18) -0.0032(16) -0.0105(15) 0.0259(19) B1 0.0141(13) 0.0160(14) 0.0146(14) -0.0019(11) -0.0015(11) 0.0064(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C47 1.750(3) . ? Fe1 C46 1.752(3) . ? Fe1 P2 2.2116(8) . ? Fe1 P1 2.2158(8) . ? Fe1 P3 2.2663(8) . ? P1 C7 1.828(3) . ? P1 C10 1.845(3) . ? P1 C16 1.851(3) . ? P2 C8 1.826(3) . ? P2 C28 1.847(3) . ? P2 C22 1.847(3) . ? P3 C9 1.825(3) . ? P3 C40 1.849(3) . ? P3 C34 1.855(3) . ? Na1 O5 2.335(3) . ? Na1 O4 2.335(3) . ? Na1 O3 2.357(3) . ? Na1 O7 2.370(2) . ? Na1 O6 2.385(3) . ? Na1 O2 2.501(2) . ? O1 C46 1.162(4) . ? O2 C47 1.158(3) . ? O3 C48 1.423(5) . ? O3 C51 1.442(5) . ? O4 C52 1.416(6) . ? O4 C55 1.442(5) . ? O5 C56 1.425(4) . ? O5 C59 1.449(4) . ? O6 C60 1.439(5) . ? O6 C63 1.449(5) . ? O7 C64 1.434(4) . ? O7 C67 1.442(4) . ? C1 C6 1.385(4) . ? C1 C2 1.394(4) . ? C1 B1 1.644(4) . ? C2 C3 1.377(5) . ? C2 H2 0.9300 . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.389(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 B1 1.664(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 B1 1.676(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 B1 1.659(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.389(4) . ? C10 C11 1.401(4) . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 C13 1.387(4) . ? C12 H12 0.9300 . ? C13 C14 1.378(5) . ? C13 H13 0.9300 . ? C14 C15 1.393(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.386(4) . ? C16 C17 1.397(4) . ? C17 C18 1.391(4) . ? C17 H17 0.9300 . ? C18 C19 1.383(4) . ? C18 H18 0.9300 . ? C19 C20 1.384(4) . ? C19 H19 0.9300 . ? C20 C21 1.392(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.395(4) . ? C22 C27 1.400(4) . ? C23 C24 1.387(4) . ? C23 H23 0.9300 . ? C24 C25 1.393(5) . ? C24 H24 0.9300 . ? C25 C26 1.375(5) . ? C25 H25 0.9300 . ? C26 C27 1.396(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.392(4) . ? C28 C33 1.395(4) . ? C29 C30 1.385(4) . ? C29 H29 0.9300 . ? C30 C31 1.394(5) . ? C30 H30 0.9300 . ? C31 C32 1.378(5) . ? C31 H31 0.9300 . ? C32 C33 1.393(4) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.391(4) . ? C34 C39 1.394(4) . ? C35 C36 1.395(4) . ? C35 H35 0.9300 . ? C36 C37 1.377(5) . ? C36 H36 0.9300 . ? C37 C38 1.381(4) . ? C37 H37 0.9300 . ? C38 C39 1.387(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.377(4) . ? C40 C45 1.404(4) . ? C41 C42 1.397(4) . ? C41 H41 0.9300 . ? C42 C43 1.367(5) . ? C42 H42 0.9300 . ? C43 C44 1.377(5) . ? C43 H43 0.9300 . ? C44 C45 1.392(4) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C48 C49 1.490(6) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.519(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.495(6) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53B 1.344(10) . ? C52 C53A 1.453(14) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53A C54A 1.52(2) . ? C53A H53A 0.9700 . ? C53A H53B 0.9700 . ? C53B C54B 1.42(4) . ? C53B H53C 0.9700 . ? C53B H53D 0.9700 . ? C54A C55 1.33(2) . ? C54A H54A 0.9700 . ? C54A H54B 0.9700 . ? C54B C55 1.61(3) . ? C54B H54C 0.9700 . ? C54B H54D 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.478(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.483(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.481(6) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.549(10) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.505(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.511(7) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.506(5) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.508(6) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.504(6) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C47 Fe1 C46 82.69(13) . . ? C47 Fe1 P2 103.94(10) . . ? C46 Fe1 P2 121.64(11) . . ? C47 Fe1 P1 93.75(9) . . ? C46 Fe1 P1 143.71(11) . . ? P2 Fe1 P1 94.35(3) . . ? C47 Fe1 P3 167.43(10) . . ? C46 Fe1 P3 89.30(9) . . ? P2 Fe1 P3 88.50(3) . . ? P1 Fe1 P3 86.97(3) . . ? C7 P1 C10 107.19(12) . . ? C7 P1 C16 102.22(12) . . ? C10 P1 C16 99.05(12) . . ? C7 P1 Fe1 113.80(9) . . ? C10 P1 Fe1 113.80(9) . . ? C16 P1 Fe1 119.03(9) . . ? C8 P2 C28 105.89(12) . . ? C8 P2 C22 103.13(12) . . ? C28 P2 C22 99.36(12) . . ? C8 P2 Fe1 114.66(9) . . ? C28 P2 Fe1 115.19(9) . . ? C22 P2 Fe1 116.73(8) . . ? C9 P3 C40 105.10(12) . . ? C9 P3 C34 104.52(12) . . ? C40 P3 C34 96.95(12) . . ? C9 P3 Fe1 114.49(9) . . ? C40 P3 Fe1 118.84(9) . . ? C34 P3 Fe1 114.67(9) . . ? O5 Na1 O4 87.23(11) . . ? O5 Na1 O3 176.77(11) . . ? O4 Na1 O3 95.33(12) . . ? O5 Na1 O7 93.89(9) . . ? O4 Na1 O7 82.37(12) . . ? O3 Na1 O7 88.40(9) . . ? O5 Na1 O6 84.36(11) . . ? O4 Na1 O6 169.43(12) . . ? O3 Na1 O6 93.30(12) . . ? O7 Na1 O6 91.82(9) . . ? O5 Na1 O2 89.73(8) . . ? O4 Na1 O2 90.59(11) . . ? O3 Na1 O2 88.29(9) . . ? O7 Na1 O2 171.90(9) . . ? O6 Na1 O2 95.75(9) . . ? C47 O2 Na1 144.4(2) . . ? C48 O3 C51 108.8(3) . . ? C48 O3 Na1 127.4(2) . . ? C51 O3 Na1 123.6(2) . . ? C52 O4 C55 106.3(4) . . ? C52 O4 Na1 122.6(3) . . ? C55 O4 Na1 130.3(3) . . ? C56 O5 C59 108.9(3) . . ? C56 O5 Na1 121.7(2) . . ? C59 O5 Na1 129.4(2) . . ? C60 O6 C63 109.8(4) . . ? C60 O6 Na1 130.6(3) . . ? C63 O6 Na1 117.7(2) . . ? C64 O7 C67 108.9(3) . . ? C64 O7 Na1 123.04(19) . . ? C67 O7 Na1 128.0(2) . . ? C6 C1 C2 114.1(3) . . ? C6 C1 B1 125.5(3) . . ? C2 C1 B1 120.3(3) . . ? C3 C2 C1 123.7(3) . . ? C3 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 118.1(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 123.5(3) . . ? C1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? B1 C7 P1 113.81(17) . . ? B1 C7 H7A 108.8 . . ? P1 C7 H7A 108.8 . . ? B1 C7 H7B 108.8 . . ? P1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? B1 C8 P2 113.63(17) . . ? B1 C8 H8A 108.8 . . ? P2 C8 H8A 108.8 . . ? B1 C8 H8B 108.8 . . ? P2 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? B1 C9 P3 112.85(18) . . ? B1 C9 H9A 109.0 . . ? P3 C9 H9A 109.0 . . ? B1 C9 H9B 109.0 . . ? P3 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C15 C10 C11 118.2(2) . . ? C15 C10 P1 126.1(2) . . ? C11 C10 P1 115.6(2) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C21 C16 C17 118.1(2) . . ? C21 C16 P1 122.6(2) . . ? C17 C16 P1 119.4(2) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.2(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 121.2(3) . . ? C16 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C27 118.0(2) . . ? C23 C22 P2 119.6(2) . . ? C27 C22 P2 122.4(2) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.5(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.6(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C29 C28 C33 118.2(3) . . ? C29 C28 P2 118.9(2) . . ? C33 C28 P2 122.8(2) . . ? C30 C29 C28 121.4(3) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.8(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C31 C32 C33 120.7(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.5(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 117.5(2) . . ? C35 C34 P3 120.4(2) . . ? C39 C34 P3 122.0(2) . . ? C34 C35 C36 121.3(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.8(3) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 121.3(3) . . ? C38 C39 H39 119.3 . . ? C34 C39 H39 119.3 . . ? C41 C40 C45 118.1(3) . . ? C41 C40 P3 123.2(2) . . ? C45 C40 P3 118.7(2) . . ? C40 C41 C42 120.9(3) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.5(3) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? O1 C46 Fe1 175.8(3) . . ? O2 C47 Fe1 174.8(2) . . ? O3 C48 C49 105.6(3) . . ? O3 C48 H48A 110.6 . . ? C49 C48 H48A 110.6 . . ? O3 C48 H48B 110.6 . . ? C49 C48 H48B 110.6 . . ? H48A C48 H48B 108.7 . . ? C48 C49 C50 101.8(4) . . ? C48 C49 H49A 111.4 . . ? C50 C49 H49A 111.4 . . ? C48 C49 H49B 111.4 . . ? C50 C49 H49B 111.4 . . ? H49A C49 H49B 109.3 . . ? C51 C50 C49 102.4(3) . . ? C51 C50 H50A 111.3 . . ? C49 C50 H50A 111.3 . . ? C51 C50 H50B 111.3 . . ? C49 C50 H50B 111.3 . . ? H50A C50 H50B 109.2 . . ? O3 C51 C50 106.9(3) . . ? O3 C51 H51A 110.3 . . ? C50 C51 H51A 110.3 . . ? O3 C51 H51B 110.3 . . ? C50 C51 H51B 110.3 . . ? H51A C51 H51B 108.6 . . ? C53B C52 O4 110.7(6) . . ? C53B C52 C53A 53.9(8) . . ? O4 C52 C53A 100.2(6) . . ? C53B C52 H52A 137.1 . . ? O4 C52 H52A 111.7 . . ? C53A C52 H52A 111.7 . . ? C53B C52 H52B 58.7 . . ? O4 C52 H52B 111.7 . . ? C53A C52 H52B 111.7 . . ? H52A C52 H52B 109.5 . . ? C52 C53A C54A 108.6(13) . . ? C52 C53A H53A 110.0 . . ? C54A C53A H53A 110.0 . . ? C52 C53A H53B 110.0 . . ? C54A C53A H53B 110.0 . . ? H53A C53A H53B 108.3 . . ? C52 C53B C54B 102.5(10) . . ? C52 C53B H53C 111.3 . . ? C54B C53B H53C 111.3 . . ? C52 C53B H53D 111.3 . . ? C54B C53B H53D 111.3 . . ? H53C C53B H53D 109.2 . . ? C55 C54A C53A 95.8(12) . . ? C55 C54A H54A 112.6 . . ? C53A C54A H54A 112.6 . . ? C55 C54A H54B 112.6 . . ? C53A C54A H54B 112.6 . . ? H54A C54A H54B 110.1 . . ? C53B C54B C55 107.9(14) . . ? C53B C54B H54C 110.1 . . ? C55 C54B H54C 110.1 . . ? C53B C54B H54D 110.1 . . ? C55 C54B H54D 110.1 . . ? H54C C54B H54D 108.4 . . ? C54A C55 O4 115.3(13) . . ? C54A C55 C54B 20.3(16) . . ? O4 C55 C54B 99.0(12) . . ? C54A C55 H55A 108.4 . . ? O4 C55 H55A 108.4 . . ? C54B C55 H55A 127.4 . . ? C54A C55 H55B 108.4 . . ? O4 C55 H55B 108.4 . . ? C54B C55 H55B 104.9 . . ? H55A C55 H55B 107.5 . . ? O5 C56 C57 107.1(3) . . ? O5 C56 H56A 110.3 . . ? C57 C56 H56A 110.3 . . ? O5 C56 H56B 110.3 . . ? C57 C56 H56B 110.3 . . ? H56A C56 H56B 108.6 . . ? C56 C57 C58 104.2(4) . . ? C56 C57 H57A 110.9 . . ? C58 C57 H57A 110.9 . . ? C56 C57 H57B 110.9 . . ? C58 C57 H57B 110.9 . . ? H57A C57 H57B 108.9 . . ? C59 C58 C57 105.1(4) . . ? C59 C58 H58A 110.7 . . ? C57 C58 H58A 110.7 . . ? C59 C58 H58B 110.7 . . ? C57 C58 H58B 110.7 . . ? H58A C58 H58B 108.8 . . ? O5 C59 C58 106.6(3) . . ? O5 C59 H59A 110.4 . . ? C58 C59 H59A 110.4 . . ? O5 C59 H59B 110.4 . . ? C58 C59 H59B 110.4 . . ? H59A C59 H59B 108.6 . . ? O6 C60 C61 102.1(5) . . ? O6 C60 H60A 111.4 . . ? C61 C60 H60A 111.4 . . ? O6 C60 H60B 111.4 . . ? C61 C60 H60B 111.4 . . ? H60A C60 H60B 109.2 . . ? C62 C61 C60 101.9(4) . . ? C62 C61 H61A 111.4 . . ? C60 C61 H61A 111.4 . . ? C62 C61 H61B 111.4 . . ? C60 C61 H61B 111.4 . . ? H61A C61 H61B 109.3 . . ? C61 C62 C63 102.7(4) . . ? C61 C62 H62A 111.2 . . ? C63 C62 H62A 111.2 . . ? C61 C62 H62B 111.2 . . ? C63 C62 H62B 111.2 . . ? H62A C62 H62B 109.1 . . ? O6 C63 C62 106.6(5) . . ? O6 C63 H63A 110.4 . . ? C62 C63 H63A 110.4 . . ? O6 C63 H63B 110.4 . . ? C62 C63 H63B 110.4 . . ? H63A C63 H63B 108.6 . . ? O7 C64 C65 106.7(3) . . ? O7 C64 H64A 110.4 . . ? C65 C64 H64A 110.4 . . ? O7 C64 H64B 110.4 . . ? C65 C64 H64B 110.4 . . ? H64A C64 H64B 108.6 . . ? C64 C65 C66 101.3(3) . . ? C64 C65 H65A 111.5 . . ? C66 C65 H65A 111.5 . . ? C64 C65 H65B 111.5 . . ? C66 C65 H65B 111.5 . . ? H65A C65 H65B 109.3 . . ? C67 C66 C65 102.4(3) . . ? C67 C66 H66A 111.3 . . ? C65 C66 H66A 111.3 . . ? C67 C66 H66B 111.3 . . ? C65 C66 H66B 111.3 . . ? H66A C66 H66B 109.2 . . ? O7 C67 C66 105.2(3) . . ? O7 C67 H67A 110.7 . . ? C66 C67 H67A 110.7 . . ? O7 C67 H67B 110.7 . . ? C66 C67 H67B 110.7 . . ? H67A C67 H67B 108.8 . . ? C1 B1 C9 107.8(2) . . ? C1 B1 C7 110.7(2) . . ? C9 B1 C7 107.4(2) . . ? C1 B1 C8 108.2(2) . . ? C9 B1 C8 108.5(2) . . ? C7 B1 C8 114.0(2) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.735 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 937864' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H82 B2 Fe2 O3 P6' _chemical_formula_weight 1542.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7605(4) _cell_length_b 16.3419(4) _cell_length_c 22.5111(6) _cell_angle_alpha 96.6650(10) _cell_angle_beta 106.7190(10) _cell_angle_gamma 103.4890(10) _cell_volume 4622.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7260 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 57.55 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 3.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2641 _exptl_absorpt_correction_T_max 0.8908 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28804 _diffrn_reflns_av_R_equivalents 0.1049 _diffrn_reflns_av_sigmaI/netI 0.1198 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 50.44 _reflns_number_total 9102 _reflns_number_gt 5692 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The dataset is 99.9 % complete to theta = 27.0. The crystals were of low-quality- attempts to grow better crystals from various solvent mixtures/temperatures did not lead to crystals that diffracted better. 4 THF molecules (per assymetric unit) were located but were so highly disordered that they could not be satisfactorily modelled. These solvent molecules were delt with by using SQUEEZE. Owing to the use of SQUEEZE, several level A alerts concerning the density are generated. There are not relevent, as the calculated density will differ from the actual density owing to the removal of 8 THF molecules. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.022 0.500 725 203 ' ' 2 0.022 0.500 1.000 366 125 ' ' _platon_squeeze_details ; The unit cell contains 8 THF molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9102 _refine_ls_number_parameters 992 _refine_ls_number_restraints 3040 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.797 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.39798(6) -0.07323(5) 0.21133(4) 0.0296(2) Uani 1 1 d U A . O1 O 0.3196(3) -0.0358(2) 0.13561(15) 0.0369(9) Uani 1 1 d U . . O2 O 0.3607(3) 0.0364(2) 0.23135(16) 0.0394(9) Uani 1 1 d U . . Fe2 Fe 0.23524(6) 0.17116(5) 0.19689(4) 0.0339(2) Uani 1 1 d U . . O3 O 0.2694(3) 0.0850(2) 0.14853(15) 0.0392(9) Uani 1 1 d U . . C46 C 0.3139(4) 0.0296(4) 0.1709(3) 0.0341(13) Uani 1 1 d U . . B1 B 0.5831(5) -0.1873(4) 0.2752(3) 0.0363(15) Uani 1 1 d DU . . C1 C 0.675(2) -0.235(2) 0.2991(8) 0.044(4) Uani 0.45(2) 1 d PDU A 1 C2 C 0.7151(15) -0.2750(14) 0.2577(9) 0.059(5) Uani 0.45(2) 1 d PDU A 1 H2 H 0.6842 -0.2782 0.2137 0.070 Uiso 0.45(2) 1 calc PR A 1 C3 C 0.7981(16) -0.3107(14) 0.2777(9) 0.070(5) Uani 0.45(2) 1 d PDU A 1 H3 H 0.8252 -0.3346 0.2477 0.083 Uiso 0.45(2) 1 calc PR A 1 C4 C 0.8410(18) -0.3118(17) 0.3400(9) 0.057(6) Uani 0.45(2) 1 d PDU A 1 H4 H 0.8995 -0.3343 0.3541 0.069 Uiso 0.45(2) 1 calc PR A 1 C5 C 0.7981(18) -0.2799(19) 0.3816(10) 0.069(6) Uani 0.45(2) 1 d PDU A 1 H5 H 0.8237 -0.2837 0.4249 0.083 Uiso 0.45(2) 1 calc PR A 1 C6 C 0.7172(16) -0.2416(16) 0.3616(9) 0.060(5) Uani 0.45(2) 1 d PDU A 1 H6 H 0.6896 -0.2192 0.3920 0.072 Uiso 0.45(2) 1 calc PR A 1 C1A C 0.6716(17) -0.2334(16) 0.3075(7) 0.038(3) Uani 0.55(2) 1 d PDU A 2 C2A C 0.6896(12) -0.3016(10) 0.2743(9) 0.061(5) Uani 0.55(2) 1 d PDU A 2 H2A H 0.6462 -0.3250 0.2317 0.073 Uiso 0.55(2) 1 calc PR A 2 C3A C 0.7704(12) -0.3368(10) 0.3024(10) 0.074(5) Uani 0.55(2) 1 d PDU A 2 H3A H 0.7805 -0.3842 0.2786 0.088 Uiso 0.55(2) 1 calc PR A 2 C4A C 0.8347(15) -0.3048(14) 0.3625(9) 0.062(5) Uani 0.55(2) 1 d PDU A 2 H4A H 0.8886 -0.3300 0.3814 0.075 Uiso 0.55(2) 1 calc PR A 2 C5A C 0.8206(13) -0.2361(14) 0.3954(7) 0.056(4) Uani 0.55(2) 1 d PDU A 2 H5A H 0.8654 -0.2126 0.4378 0.067 Uiso 0.55(2) 1 calc PR A 2 C6A C 0.7416(12) -0.1998(13) 0.3679(7) 0.052(4) Uani 0.55(2) 1 d PDU A 2 H6A H 0.7354 -0.1501 0.3913 0.063 Uiso 0.55(2) 1 calc PR A 2 C7 C 0.5139(4) -0.1770(3) 0.3242(2) 0.0388(14) Uani 1 1 d DU A . H7A H 0.5622 -0.1619 0.3685 0.047 Uiso 1 1 calc R . . H7B H 0.4614 -0.2326 0.3190 0.047 Uiso 1 1 calc R . . P1 P 0.44623(11) -0.09537(9) 0.30920(6) 0.0343(4) Uani 1 1 d DU . . C10 C 0.5273(4) -0.0016(3) 0.3697(2) 0.0356(13) Uani 1 1 d DU A . C11 C 0.5617(4) -0.0085(3) 0.4341(2) 0.0433(15) Uani 1 1 d DU . . H11 H 0.5427 -0.0627 0.4455 0.052 Uiso 1 1 calc R A . C12 C 0.6220(4) 0.0624(4) 0.4800(3) 0.0509(16) Uani 1 1 d DU A . H12 H 0.6450 0.0561 0.5228 0.061 Uiso 1 1 calc R . . C13 C 0.6504(4) 0.1425(4) 0.4659(3) 0.0553(17) Uani 1 1 d DU . . H13 H 0.6921 0.1909 0.4984 0.066 Uiso 1 1 calc R A . C14 C 0.6170(4) 0.1511(3) 0.4032(2) 0.0453(15) Uani 1 1 d DU A . H14 H 0.6351 0.2057 0.3922 0.054 Uiso 1 1 calc R . . C15 C 0.5568(4) 0.0790(3) 0.3567(2) 0.0386(14) Uani 1 1 d DU . . H15 H 0.5349 0.0857 0.3139 0.046 Uiso 1 1 calc R A . C16 C 0.3295(4) -0.1220(3) 0.3348(2) 0.0322(13) Uani 1 1 d DU A . C17 C 0.2946(4) -0.1998(3) 0.3527(2) 0.0397(14) Uani 1 1 d DU . . H17 H 0.3335 -0.2409 0.3540 0.048 Uiso 1 1 calc R A . C18 C 0.2023(4) -0.2164(4) 0.3688(2) 0.0458(15) Uani 1 1 d DU A . H18 H 0.1780 -0.2697 0.3803 0.055 Uiso 1 1 calc R . . C19 C 0.1462(4) -0.1572(4) 0.3683(3) 0.0491(16) Uani 1 1 d DU . . H19 H 0.0839 -0.1693 0.3798 0.059 Uiso 1 1 calc R A . C20 C 0.1802(4) -0.0799(4) 0.3511(3) 0.0489(16) Uani 1 1 d DU A . H20 H 0.1419 -0.0385 0.3512 0.059 Uiso 1 1 calc R . . C21 C 0.2710(4) -0.0629(3) 0.3334(2) 0.0420(14) Uani 1 1 d DU . . H21 H 0.2932 -0.0104 0.3202 0.050 Uiso 1 1 calc R A . C8 C 0.4992(3) -0.2450(3) 0.2078(2) 0.0375(13) Uani 1 1 d DU A . H8A H 0.4760 -0.3049 0.2133 0.045 Uiso 1 1 calc R . . H8B H 0.5365 -0.2454 0.1762 0.045 Uiso 1 1 calc R . . P2 P 0.38197(10) -0.20859(9) 0.17626(6) 0.0334(4) Uani 1 1 d DU . . C22 C 0.2745(4) -0.2766(3) 0.1967(2) 0.0346(13) Uani 1 1 d DU A . C23 C 0.1868(4) -0.2461(3) 0.1949(2) 0.0409(14) Uani 1 1 d DU . . H23 H 0.1847 -0.1922 0.1834 0.049 Uiso 1 1 calc R A . C24 C 0.1026(4) -0.2943(4) 0.2098(2) 0.0443(15) Uani 1 1 d DU A . H24 H 0.0444 -0.2723 0.2095 0.053 Uiso 1 1 calc R . . C25 C 0.1027(4) -0.3728(4) 0.2249(3) 0.0538(17) Uani 1 1 d DU . . H25 H 0.0441 -0.4058 0.2342 0.065 Uiso 1 1 calc R A . C26 C 0.1878(5) -0.4037(4) 0.2267(3) 0.0589(18) Uani 1 1 d DU A . H26 H 0.1882 -0.4581 0.2376 0.071 Uiso 1 1 calc R . . C27 C 0.2733(4) -0.3560(3) 0.2128(3) 0.0510(16) Uani 1 1 d DU . . H27 H 0.3317 -0.3782 0.2143 0.061 Uiso 1 1 calc R A . C28 C 0.3345(4) -0.2469(3) 0.0901(2) 0.0356(13) Uani 1 1 d DU A . C29 C 0.2498(4) -0.2223(3) 0.0522(2) 0.0380(14) Uani 1 1 d DU . . H29 H 0.2167 -0.1872 0.0715 0.046 Uiso 1 1 calc R A . C30 C 0.2138(4) -0.2485(3) -0.0130(2) 0.0437(15) Uani 1 1 d DU A . H30 H 0.1564 -0.2313 -0.0379 0.052 Uiso 1 1 calc R . . C31 C 0.2612(4) -0.2997(4) -0.0421(3) 0.0469(16) Uani 1 1 d DU . . H31 H 0.2367 -0.3173 -0.0868 0.056 Uiso 1 1 calc R A . C32 C 0.3444(4) -0.3249(4) -0.0056(3) 0.0533(16) Uani 1 1 d DU A . H32 H 0.3767 -0.3604 -0.0252 0.064 Uiso 1 1 calc R . . C33 C 0.3803(4) -0.2987(3) 0.0589(2) 0.0400(14) Uani 1 1 d DU . . H33 H 0.4379 -0.3161 0.0833 0.048 Uiso 1 1 calc R A . C9 C 0.6424(4) -0.0897(3) 0.2662(2) 0.0353(13) Uani 1 1 d DU A . H9A H 0.7045 -0.0930 0.2532 0.042 Uiso 1 1 calc R . . H9B H 0.6683 -0.0497 0.3075 0.042 Uiso 1 1 calc R . . P3 P 0.55752(10) -0.04688(9) 0.20862(6) 0.0311(4) Uani 1 1 d DU . . C34 C 0.5664(4) -0.0881(3) 0.1311(2) 0.0296(12) Uani 1 1 d DU A . C35 C 0.4933(4) -0.0794(3) 0.0763(2) 0.0346(13) Uani 1 1 d DU . . H35 H 0.4400 -0.0529 0.0796 0.041 Uiso 1 1 calc R A . C36 C 0.4974(4) -0.1090(3) 0.0169(2) 0.0390(14) Uani 1 1 d DU A . H36 H 0.4474 -0.1018 -0.0198 0.047 Uiso 1 1 calc R . . C37 C 0.5724(4) -0.1483(4) 0.0105(2) 0.0468(16) Uani 1 1 d DU . . H37 H 0.5748 -0.1683 -0.0303 0.056 Uiso 1 1 calc R A . C38 C 0.6450(4) -0.1586(4) 0.0646(3) 0.0510(16) Uani 1 1 d DU A . H38 H 0.6962 -0.1872 0.0608 0.061 Uiso 1 1 calc R . . C39 C 0.6429(4) -0.1270(3) 0.1244(2) 0.0400(14) Uani 1 1 d DU . . H39 H 0.6947 -0.1323 0.1610 0.048 Uiso 1 1 calc R A . C40 C 0.6220(4) 0.0663(3) 0.2168(2) 0.0337(13) Uani 1 1 d DU A . C41 C 0.7198(4) 0.1085(3) 0.2611(2) 0.0381(14) Uani 1 1 d DU . . H41 H 0.7536 0.0785 0.2906 0.046 Uiso 1 1 calc R A . C42 C 0.7696(4) 0.1936(4) 0.2636(3) 0.0499(16) Uani 1 1 d DU A . H42 H 0.8359 0.2213 0.2953 0.060 Uiso 1 1 calc R . . C43 C 0.7238(5) 0.2382(4) 0.2207(3) 0.0556(17) Uani 1 1 d DU . . H43 H 0.7590 0.2960 0.2218 0.067 Uiso 1 1 calc R A . C44 C 0.6266(5) 0.1982(4) 0.1761(3) 0.0510(16) Uani 1 1 d DU A . H44 H 0.5939 0.2288 0.1466 0.061 Uiso 1 1 calc R . . C45 C 0.5763(4) 0.1136(3) 0.1740(2) 0.0388(14) Uani 1 1 d DU . . H45 H 0.5093 0.0868 0.1428 0.047 Uiso 1 1 calc R A . B2 B 0.1085(5) 0.3284(4) 0.2343(3) 0.0396(16) Uani 1 1 d U . . C47 C 0.0422(5) 0.3918(3) 0.2525(3) 0.0435(14) Uani 1 1 d U . . C48 C -0.0448(5) 0.4030(4) 0.2061(3) 0.0548(16) Uani 1 1 d U . . H48 H -0.0582 0.3782 0.1632 0.066 Uiso 1 1 calc R . . C49 C -0.1128(5) 0.4489(4) 0.2198(3) 0.0659(19) Uani 1 1 d U . . H49 H -0.1706 0.4550 0.1870 0.079 Uiso 1 1 calc R . . C50 C -0.0939(6) 0.4848(4) 0.2817(4) 0.074(2) Uani 1 1 d U . . H50 H -0.1394 0.5154 0.2922 0.089 Uiso 1 1 calc R . . C51 C -0.0099(7) 0.4766(5) 0.3282(4) 0.090(3) Uani 1 1 d U . . H51 H 0.0035 0.5018 0.3711 0.108 Uiso 1 1 calc R . . C52 C 0.0559(6) 0.4313(4) 0.3128(3) 0.072(2) Uani 1 1 d U . . H52 H 0.1143 0.4274 0.3461 0.087 Uiso 1 1 calc R . . C53 C 0.0995(4) 0.3210(3) 0.1586(2) 0.0342(13) Uani 1 1 d DU . . H53A H 0.1091 0.3795 0.1492 0.041 Uiso 1 1 calc R . . H53B H 0.0267 0.2870 0.1328 0.041 Uiso 1 1 calc R . . P4 P 0.19014(11) 0.27405(9) 0.13177(6) 0.0346(4) Uani 1 1 d DU . . C56 C 0.1314(4) 0.2432(3) 0.0456(2) 0.0365(13) Uani 1 1 d DU . . C57 C 0.0633(4) 0.2856(3) 0.0122(2) 0.0423(14) Uani 1 1 d DU . . H57 H 0.0492 0.3325 0.0341 0.051 Uiso 1 1 calc R . . C58 C 0.0164(4) 0.2602(3) -0.0522(2) 0.0455(15) Uani 1 1 d DU . . H58 H -0.0303 0.2893 -0.0744 0.055 Uiso 1 1 calc R . . C59 C 0.0367(4) 0.1925(3) -0.0850(2) 0.0417(15) Uani 1 1 d DU . . H59 H 0.0036 0.1749 -0.1294 0.050 Uiso 1 1 calc R . . C60 C 0.1057(4) 0.1507(3) -0.0524(2) 0.0403(14) Uani 1 1 d DU . . H60 H 0.1201 0.1043 -0.0746 0.048 Uiso 1 1 calc R . . C61 C 0.1535(4) 0.1766(3) 0.0122(2) 0.0333(13) Uani 1 1 d DU . . H61 H 0.2019 0.1486 0.0342 0.040 Uiso 1 1 calc R . . C62 C 0.3104(4) 0.3575(3) 0.1419(2) 0.0343(13) Uani 1 1 d DU . . C63 C 0.3143(4) 0.4422(3) 0.1370(3) 0.0517(16) Uani 1 1 d DU . . H63 H 0.2510 0.4592 0.1292 0.062 Uiso 1 1 calc R . . C64 C 0.4078(5) 0.5024(4) 0.1432(3) 0.0629(18) Uani 1 1 d DU . . H64 H 0.4082 0.5599 0.1398 0.076 Uiso 1 1 calc R . . C65 C 0.5005(5) 0.4784(4) 0.1543(3) 0.072(2) Uani 1 1 d DU . . H65 H 0.5654 0.5195 0.1597 0.086 Uiso 1 1 calc R . . C66 C 0.4976(5) 0.3941(4) 0.1574(3) 0.0572(17) Uani 1 1 d DU . . H66 H 0.5607 0.3770 0.1640 0.069 Uiso 1 1 calc R . . C67 C 0.4050(4) 0.3348(3) 0.1513(2) 0.0457(15) Uani 1 1 d DU . . H67 H 0.4049 0.2770 0.1533 0.055 Uiso 1 1 calc R . . C54 C 0.2357(4) 0.3670(3) 0.2788(2) 0.0400(14) Uani 1 1 d DU . . H54A H 0.2390 0.3943 0.3212 0.048 Uiso 1 1 calc R . . H54B H 0.2697 0.4126 0.2600 0.048 Uiso 1 1 calc R . . P5 P 0.31352(11) 0.29114(9) 0.28906(7) 0.0398(4) Uani 1 1 d DU . . C68 C 0.4524(4) 0.3528(4) 0.3109(2) 0.0414(14) Uani 1 1 d DU . . C69 C 0.5285(4) 0.3105(4) 0.3069(2) 0.0498(15) Uani 1 1 d DU . . H69 H 0.5078 0.2500 0.2928 0.060 Uiso 1 1 calc R . . C70 C 0.6335(4) 0.3562(4) 0.3233(3) 0.0609(18) Uani 1 1 d DU . . H70 H 0.6850 0.3268 0.3217 0.073 Uiso 1 1 calc R . . C71 C 0.6637(5) 0.4437(4) 0.3418(3) 0.067(2) Uani 1 1 d DU . . H71 H 0.7360 0.4748 0.3530 0.081 Uiso 1 1 calc R . . C72 C 0.5888(5) 0.4871(4) 0.3444(3) 0.077(2) Uani 1 1 d DU . . H72 H 0.6092 0.5478 0.3564 0.093 Uiso 1 1 calc R . . C73 C 0.4850(4) 0.4406(4) 0.3293(3) 0.0606(18) Uani 1 1 d DU . . H73 H 0.4340 0.4702 0.3317 0.073 Uiso 1 1 calc R . . C74 C 0.3097(4) 0.2499(3) 0.3611(2) 0.0412(14) Uani 1 1 d DU . . C75 C 0.3431(4) 0.1780(3) 0.3702(3) 0.0502(16) Uani 1 1 d DU . . H75 H 0.3630 0.1497 0.3382 0.060 Uiso 1 1 calc R . . C76 C 0.3485(5) 0.1459(4) 0.4248(3) 0.0608(18) Uani 1 1 d DU . . H76 H 0.3741 0.0972 0.4309 0.073 Uiso 1 1 calc R . . C77 C 0.3163(5) 0.1852(4) 0.4704(3) 0.068(2) Uani 1 1 d DU . . H77 H 0.3164 0.1620 0.5072 0.082 Uiso 1 1 calc R . . C78 C 0.2838(5) 0.2578(4) 0.4624(3) 0.069(2) Uani 1 1 d DU . . H78 H 0.2639 0.2857 0.4946 0.083 Uiso 1 1 calc R . . C79 C 0.2798(4) 0.2913(4) 0.4076(3) 0.0593(18) Uani 1 1 d DU . . H79 H 0.2570 0.3414 0.4023 0.071 Uiso 1 1 calc R . . C55 C 0.0528(4) 0.2351(3) 0.2492(2) 0.0382(13) Uani 1 1 d DU . . H55A H -0.0236 0.2299 0.2389 0.046 Uiso 1 1 calc R . . H55B H 0.0813 0.2388 0.2954 0.046 Uiso 1 1 calc R . . P6 P 0.06433(11) 0.13582(9) 0.21138(6) 0.0355(4) Uani 1 1 d DU . . C80 C -0.0429(4) 0.1018(3) 0.1356(2) 0.0333(13) Uani 1 1 d DU . . C81 C -0.0224(4) 0.0808(3) 0.0795(2) 0.0372(14) Uani 1 1 d DU . . H81 H 0.0483 0.0862 0.0804 0.045 Uiso 1 1 calc R . . C82 C -0.1040(4) 0.0523(3) 0.0224(2) 0.0395(14) Uani 1 1 d DU . . H82 H -0.0887 0.0405 -0.0157 0.047 Uiso 1 1 calc R . . C83 C -0.2073(4) 0.0408(3) 0.0205(2) 0.0421(15) Uani 1 1 d DU . . H83 H -0.2631 0.0209 -0.0187 0.051 Uiso 1 1 calc R . . C84 C -0.2290(4) 0.0585(3) 0.0762(2) 0.0401(14) Uani 1 1 d DU . . H84 H -0.3003 0.0495 0.0751 0.048 Uiso 1 1 calc R . . C85 C -0.1480(4) 0.0892(3) 0.1335(2) 0.0383(14) Uani 1 1 d DU . . H85 H -0.1638 0.1017 0.1713 0.046 Uiso 1 1 calc R . . C86 C 0.0171(4) 0.0514(3) 0.2511(2) 0.0348(13) Uani 1 1 d DU . . C87 C -0.0098(4) -0.0322(3) 0.2215(3) 0.0525(16) Uani 1 1 d DU . . H87 H 0.0041 -0.0442 0.1829 0.063 Uiso 1 1 calc R . . C88 C -0.0555(5) -0.0999(4) 0.2442(3) 0.072(2) Uani 1 1 d DU . . H88 H -0.0710 -0.1571 0.2224 0.086 Uiso 1 1 calc R . . C89 C -0.0789(5) -0.0837(4) 0.2993(3) 0.070(2) Uani 1 1 d DU . . H89 H -0.1124 -0.1295 0.3155 0.084 Uiso 1 1 calc R . . C90 C -0.0531(5) -0.0009(5) 0.3300(3) 0.074(2) Uani 1 1 d DU . . H90 H -0.0686 0.0108 0.3680 0.089 Uiso 1 1 calc R . . C91 C -0.0041(4) 0.0677(4) 0.3066(3) 0.0626(18) Uani 1 1 d DU . . H91 H 0.0143 0.1249 0.3291 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0264(5) 0.0328(6) 0.0310(5) 0.0078(4) 0.0096(4) 0.0095(4) O1 0.039(2) 0.038(2) 0.035(2) 0.0101(18) 0.0070(17) 0.019(2) O2 0.039(2) 0.041(2) 0.033(2) 0.0045(17) 0.0055(18) 0.0117(19) Fe2 0.0348(5) 0.0353(6) 0.0325(5) 0.0054(4) 0.0111(4) 0.0120(5) O3 0.041(2) 0.044(2) 0.041(2) 0.0102(18) 0.0140(18) 0.026(2) C46 0.026(3) 0.027(3) 0.046(3) 0.002(3) 0.011(3) 0.007(3) B1 0.034(4) 0.035(4) 0.045(4) 0.011(3) 0.012(3) 0.017(3) C1 0.036(8) 0.041(8) 0.056(8) 0.017(8) 0.009(7) 0.016(7) C2 0.087(10) 0.052(11) 0.065(9) 0.036(8) 0.026(7) 0.058(8) C3 0.091(11) 0.080(12) 0.069(10) 0.038(9) 0.033(8) 0.063(9) C4 0.040(10) 0.060(11) 0.056(11) -0.005(10) -0.009(9) 0.024(8) C5 0.053(11) 0.106(16) 0.059(10) 0.026(11) 0.011(8) 0.046(11) C6 0.037(10) 0.090(14) 0.054(8) 0.013(9) 0.006(7) 0.032(9) C1A 0.031(7) 0.049(7) 0.047(7) 0.024(6) 0.020(5) 0.018(6) C2A 0.065(9) 0.051(9) 0.064(9) 0.015(6) -0.005(6) 0.043(7) C3A 0.074(10) 0.066(9) 0.086(12) 0.021(8) 0.005(8) 0.054(8) C4A 0.043(9) 0.078(11) 0.072(12) 0.041(9) 0.006(8) 0.031(7) C5A 0.039(8) 0.091(12) 0.041(8) 0.030(7) 0.012(6) 0.016(8) C6A 0.043(8) 0.072(11) 0.049(6) 0.019(6) 0.016(5) 0.024(8) C7 0.034(3) 0.041(4) 0.047(4) 0.017(3) 0.015(3) 0.015(3) P1 0.0322(9) 0.0369(10) 0.0367(9) 0.0122(7) 0.0117(7) 0.0124(8) C10 0.030(3) 0.039(3) 0.043(3) 0.012(3) 0.017(3) 0.012(3) C11 0.040(4) 0.042(4) 0.043(3) 0.014(3) 0.011(3) 0.003(3) C12 0.051(4) 0.051(4) 0.036(4) 0.006(3) 0.003(3) 0.000(3) C13 0.051(4) 0.050(4) 0.039(4) -0.001(3) -0.004(3) -0.006(3) C14 0.046(4) 0.042(4) 0.041(4) 0.008(3) 0.013(3) 0.002(3) C15 0.037(3) 0.043(4) 0.032(3) 0.005(3) 0.012(3) 0.004(3) C16 0.027(3) 0.039(4) 0.031(3) 0.010(3) 0.010(2) 0.009(3) C17 0.039(3) 0.036(4) 0.045(4) 0.009(3) 0.016(3) 0.009(3) C18 0.046(4) 0.042(4) 0.042(4) 0.012(3) 0.013(3) 0.000(3) C19 0.031(4) 0.068(5) 0.051(4) 0.017(3) 0.015(3) 0.014(3) C20 0.038(4) 0.058(4) 0.060(4) 0.023(3) 0.017(3) 0.024(3) C21 0.030(3) 0.048(4) 0.049(4) 0.017(3) 0.011(3) 0.013(3) C8 0.031(3) 0.048(4) 0.043(3) 0.020(3) 0.014(2) 0.021(3) P2 0.0280(8) 0.0352(10) 0.0384(9) 0.0098(7) 0.0118(7) 0.0087(8) C22 0.030(3) 0.026(3) 0.041(3) 0.006(3) 0.011(3) -0.003(3) C23 0.035(3) 0.043(4) 0.040(4) 0.010(3) 0.007(3) 0.006(3) C24 0.030(3) 0.053(4) 0.045(4) 0.009(3) 0.013(3) 0.002(3) C25 0.043(4) 0.047(4) 0.064(4) 0.008(3) 0.024(3) -0.008(3) C26 0.076(5) 0.036(4) 0.073(5) 0.017(3) 0.043(4) 0.006(4) C27 0.050(4) 0.031(4) 0.079(5) 0.012(3) 0.034(3) 0.006(3) C28 0.037(3) 0.037(4) 0.036(3) 0.011(3) 0.016(2) 0.008(3) C29 0.031(3) 0.041(4) 0.042(3) 0.008(3) 0.012(3) 0.008(3) C30 0.028(3) 0.050(4) 0.045(4) 0.011(3) 0.003(3) 0.007(3) C31 0.040(4) 0.061(5) 0.037(4) 0.006(3) 0.015(3) 0.007(3) C32 0.050(4) 0.062(5) 0.053(4) 0.002(3) 0.023(3) 0.021(4) C33 0.041(4) 0.035(4) 0.040(3) 0.000(3) 0.008(3) 0.014(3) C9 0.036(3) 0.047(4) 0.029(3) 0.015(3) 0.010(2) 0.020(3) P3 0.0293(8) 0.0349(10) 0.0321(9) 0.0090(7) 0.0110(7) 0.0121(7) C34 0.030(3) 0.030(3) 0.030(3) 0.005(2) 0.013(2) 0.009(3) C35 0.030(3) 0.043(4) 0.035(3) 0.012(3) 0.013(3) 0.013(3) C36 0.030(3) 0.051(4) 0.032(3) 0.010(3) 0.006(3) 0.008(3) C37 0.043(4) 0.068(5) 0.036(4) 0.010(3) 0.020(3) 0.018(3) C38 0.045(4) 0.074(5) 0.052(4) 0.014(3) 0.029(3) 0.032(3) C39 0.035(3) 0.051(4) 0.037(3) 0.007(3) 0.013(3) 0.017(3) C40 0.032(3) 0.042(3) 0.029(3) 0.003(3) 0.012(2) 0.014(3) C41 0.041(3) 0.039(4) 0.039(4) 0.005(3) 0.020(3) 0.012(3) C42 0.040(4) 0.050(4) 0.053(4) -0.005(3) 0.019(3) 0.001(3) C43 0.071(4) 0.037(4) 0.062(5) 0.006(3) 0.042(3) -0.001(3) C44 0.070(4) 0.040(4) 0.047(4) 0.012(3) 0.024(3) 0.015(4) C45 0.042(4) 0.033(3) 0.045(4) 0.007(3) 0.019(3) 0.012(3) B2 0.049(4) 0.038(4) 0.041(4) 0.010(3) 0.021(3) 0.020(3) C47 0.054(4) 0.033(4) 0.055(4) 0.007(3) 0.033(3) 0.015(3) C48 0.049(4) 0.042(4) 0.079(4) -0.001(3) 0.034(3) 0.012(3) C49 0.060(4) 0.039(4) 0.115(5) 0.016(4) 0.052(4) 0.015(4) C50 0.104(6) 0.057(5) 0.117(6) 0.040(5) 0.091(5) 0.047(5) C51 0.153(8) 0.092(6) 0.078(5) 0.027(5) 0.076(5) 0.082(6) C52 0.109(6) 0.080(5) 0.057(4) 0.019(4) 0.042(4) 0.058(5) C53 0.037(3) 0.028(3) 0.046(3) 0.009(3) 0.020(3) 0.016(3) P4 0.0354(9) 0.0326(10) 0.0368(9) 0.0045(7) 0.0127(7) 0.0118(8) C56 0.037(3) 0.037(4) 0.038(3) 0.009(3) 0.011(3) 0.013(3) C57 0.043(4) 0.049(4) 0.035(3) 0.006(3) 0.010(3) 0.018(3) C58 0.045(4) 0.046(4) 0.044(4) 0.009(3) 0.006(3) 0.021(3) C59 0.054(4) 0.037(4) 0.037(4) 0.010(3) 0.017(3) 0.016(3) C60 0.045(4) 0.042(4) 0.043(4) 0.009(3) 0.019(3) 0.023(3) C61 0.029(3) 0.035(4) 0.036(3) 0.009(3) 0.006(3) 0.014(3) C62 0.043(3) 0.023(3) 0.037(3) 0.002(3) 0.017(3) 0.006(3) C63 0.051(4) 0.036(4) 0.062(4) 0.003(3) 0.021(3) 0.002(3) C64 0.070(4) 0.032(4) 0.083(5) -0.001(3) 0.035(4) 0.000(3) C65 0.063(4) 0.056(4) 0.099(6) 0.004(4) 0.050(4) -0.001(4) C66 0.051(4) 0.062(5) 0.065(4) 0.015(4) 0.032(3) 0.012(4) C67 0.041(3) 0.044(4) 0.057(4) 0.014(3) 0.023(3) 0.012(3) C54 0.057(3) 0.030(3) 0.043(4) 0.008(3) 0.023(3) 0.023(3) P5 0.0451(10) 0.0389(10) 0.0373(10) 0.0053(7) 0.0162(7) 0.0129(8) C68 0.034(3) 0.052(4) 0.034(4) 0.009(3) 0.011(3) 0.005(3) C69 0.046(3) 0.060(4) 0.039(4) 0.011(3) 0.009(3) 0.013(3) C70 0.045(4) 0.077(5) 0.061(5) 0.014(4) 0.025(3) 0.008(4) C71 0.041(4) 0.086(5) 0.066(5) 0.010(4) 0.019(3) -0.001(4) C72 0.054(4) 0.067(5) 0.098(6) 0.006(4) 0.027(4) -0.004(4) C73 0.043(4) 0.056(4) 0.069(5) -0.004(4) 0.017(3) -0.003(3) C74 0.041(4) 0.047(4) 0.038(3) 0.008(3) 0.016(3) 0.013(3) C75 0.066(4) 0.048(4) 0.044(4) 0.014(3) 0.025(3) 0.019(3) C76 0.077(5) 0.055(5) 0.053(4) 0.015(3) 0.018(4) 0.026(4) C77 0.089(5) 0.084(5) 0.052(4) 0.027(4) 0.033(4) 0.043(4) C78 0.096(5) 0.088(5) 0.052(4) 0.028(4) 0.044(4) 0.049(5) C79 0.072(5) 0.078(5) 0.045(4) 0.019(3) 0.026(3) 0.042(4) C55 0.038(3) 0.040(3) 0.034(3) -0.001(3) 0.007(3) 0.014(3) P6 0.0369(9) 0.0342(10) 0.0372(9) 0.0071(7) 0.0132(7) 0.0120(8) C80 0.038(3) 0.022(3) 0.043(3) 0.008(3) 0.017(3) 0.007(3) C81 0.037(3) 0.039(4) 0.040(3) 0.009(3) 0.020(3) 0.010(3) C82 0.049(4) 0.041(4) 0.036(3) 0.010(3) 0.020(3) 0.016(3) C83 0.038(3) 0.050(4) 0.032(3) 0.006(3) 0.004(3) 0.012(3) C84 0.033(3) 0.048(4) 0.042(4) 0.015(3) 0.010(3) 0.016(3) C85 0.039(3) 0.043(4) 0.039(3) 0.012(3) 0.018(3) 0.014(3) C86 0.023(3) 0.040(3) 0.040(3) 0.009(3) 0.006(3) 0.011(3) C87 0.056(4) 0.036(4) 0.046(4) 0.015(3) -0.005(3) 0.000(4) C88 0.054(4) 0.062(5) 0.080(5) 0.035(4) -0.005(4) 0.003(4) C89 0.031(4) 0.079(5) 0.121(6) 0.066(5) 0.030(4) 0.025(4) C90 0.070(5) 0.105(6) 0.100(6) 0.064(5) 0.060(4) 0.062(5) C91 0.071(5) 0.065(4) 0.080(5) 0.035(4) 0.046(4) 0.036(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.984(3) . ? Fe1 O2 2.013(3) . ? Fe1 P3 2.1567(15) . ? Fe1 P2 2.1983(16) . ? Fe1 P1 2.2092(15) . ? Fe1 C46 2.376(6) . ? O1 C46 1.288(6) . ? O2 C46 1.305(6) . ? Fe2 O3 1.907(3) . ? Fe2 P6 2.4128(16) . ? Fe2 P4 2.4283(16) . ? Fe2 P5 2.4687(17) . ? O3 C46 1.279(6) . ? B1 C1A 1.620(11) . ? B1 C1 1.635(12) . ? B1 C8 1.636(7) . ? B1 C7 1.671(7) . ? B1 C9 1.676(7) . ? C1 C2 1.384(12) . ? C1 C6 1.386(12) . ? C2 C3 1.386(12) . ? C2 H2 0.9500 . ? C3 C4 1.360(12) . ? C3 H3 0.9500 . ? C4 C5 1.358(13) . ? C4 H4 0.9500 . ? C5 C6 1.391(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C1A C6A 1.380(12) . ? C1A C2A 1.381(11) . ? C2A C3A 1.394(11) . ? C2A H2A 0.9500 . ? C3A C4A 1.348(12) . ? C3A H3A 0.9500 . ? C4A C5A 1.356(12) . ? C4A H4A 0.9500 . ? C5A C6A 1.385(11) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7 P1 1.807(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? P1 C10 1.815(5) . ? P1 C16 1.834(4) . ? C10 C15 1.376(6) . ? C10 C11 1.415(6) . ? C11 C12 1.371(6) . ? C11 H11 0.9500 . ? C12 C13 1.378(6) . ? C12 H12 0.9500 . ? C13 C14 1.386(6) . ? C13 H13 0.9500 . ? C14 C15 1.390(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.393(6) . ? C16 C17 1.397(6) . ? C17 C18 1.394(6) . ? C17 H17 0.9500 . ? C18 C19 1.371(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C8 P2 1.830(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P2 C22 1.837(4) . ? P2 C28 1.839(5) . ? C22 C27 1.386(6) . ? C22 C23 1.401(6) . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 C25 1.364(6) . ? C24 H24 0.9500 . ? C25 C26 1.372(6) . ? C25 H25 0.9500 . ? C26 C27 1.391(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.403(6) . ? C28 C29 1.406(6) . ? C29 C30 1.385(6) . ? C29 H29 0.9500 . ? C30 C31 1.389(6) . ? C30 H30 0.9500 . ? C31 C32 1.383(6) . ? C31 H31 0.9500 . ? C32 C33 1.371(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C9 P3 1.804(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? P3 C40 1.817(5) . ? P3 C34 1.845(4) . ? C34 C39 1.384(5) . ? C34 C35 1.395(6) . ? C35 C36 1.389(6) . ? C35 H35 0.9500 . ? C36 C37 1.368(6) . ? C36 H36 0.9500 . ? C37 C38 1.391(6) . ? C37 H37 0.9500 . ? C38 C39 1.395(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.385(6) . ? C40 C45 1.404(6) . ? C41 C42 1.386(6) . ? C41 H41 0.9500 . ? C42 C43 1.375(6) . ? C42 H42 0.9500 . ? C43 C44 1.375(6) . ? C43 H43 0.9500 . ? C44 C45 1.384(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? B2 C47 1.622(8) . ? B2 C55 1.657(7) . ? B2 C53 1.662(7) . ? B2 C54 1.671(8) . ? C47 C52 1.374(7) . ? C47 C48 1.408(7) . ? C48 C49 1.405(7) . ? C48 H48 0.9500 . ? C49 C50 1.373(8) . ? C49 H49 0.9500 . ? C50 C51 1.363(9) . ? C50 H50 0.9500 . ? C51 C52 1.386(8) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 P4 1.811(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? P4 C62 1.818(5) . ? P4 C56 1.831(5) . ? C56 C61 1.392(6) . ? C56 C57 1.394(6) . ? C57 C58 1.373(6) . ? C57 H57 0.9500 . ? C58 C59 1.385(6) . ? C58 H58 0.9500 . ? C59 C60 1.387(6) . ? C59 H59 0.9500 . ? C60 C61 1.380(6) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.391(6) . ? C62 C67 1.401(6) . ? C63 C64 1.385(6) . ? C63 H63 0.9500 . ? C64 C65 1.385(7) . ? C64 H64 0.9500 . ? C65 C66 1.380(6) . ? C65 H65 0.9500 . ? C66 C67 1.368(6) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C54 P5 1.811(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? P5 C68 1.831(5) . ? P5 C74 1.835(5) . ? C68 C73 1.373(6) . ? C68 C69 1.401(6) . ? C69 C70 1.381(6) . ? C69 H69 0.9500 . ? C70 C71 1.369(7) . ? C70 H70 0.9500 . ? C71 C72 1.390(7) . ? C71 H71 0.9500 . ? C72 C73 1.375(6) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C74 C75 1.374(6) . ? C74 C79 1.393(6) . ? C75 C76 1.381(6) . ? C75 H75 0.9500 . ? C76 C77 1.379(6) . ? C76 H76 0.9500 . ? C77 C78 1.376(6) . ? C77 H77 0.9500 . ? C78 C79 1.398(6) . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? C55 P6 1.805(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? P6 C86 1.823(5) . ? P6 C80 1.829(5) . ? C80 C81 1.395(6) . ? C80 C85 1.398(6) . ? C81 C82 1.384(6) . ? C81 H81 0.9500 . ? C82 C83 1.376(6) . ? C82 H82 0.9500 . ? C83 C84 1.383(6) . ? C83 H83 0.9500 . ? C84 C85 1.386(6) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 C87 1.364(6) . ? C86 C91 1.374(6) . ? C87 C88 1.368(6) . ? C87 H87 0.9500 . ? C88 C89 1.381(7) . ? C88 H88 0.9500 . ? C89 C90 1.360(7) . ? C89 H89 0.9500 . ? C90 C91 1.406(7) . ? C90 H90 0.9500 . ? C91 H91 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 66.14(14) . . ? O1 Fe1 P3 104.33(10) . . ? O2 Fe1 P3 110.96(10) . . ? O1 Fe1 P2 103.63(11) . . ? O2 Fe1 P2 161.14(11) . . ? P3 Fe1 P2 86.54(6) . . ? O1 Fe1 P1 159.22(11) . . ? O2 Fe1 P1 96.68(10) . . ? P3 Fe1 P1 92.48(5) . . ? P2 Fe1 P1 89.27(6) . . ? O1 Fe1 C46 32.83(15) . . ? O2 Fe1 C46 33.32(14) . . ? P3 Fe1 C46 111.68(13) . . ? P2 Fe1 C46 134.41(14) . . ? P1 Fe1 C46 128.93(14) . . ? C46 O1 Fe1 90.6(3) . . ? C46 O2 Fe1 88.8(3) . . ? O3 Fe2 P6 117.97(11) . . ? O3 Fe2 P4 108.57(11) . . ? P6 Fe2 P4 92.41(5) . . ? O3 Fe2 P5 142.42(11) . . ? P6 Fe2 P5 93.86(5) . . ? P4 Fe2 P5 88.07(5) . . ? C46 O3 Fe2 125.2(3) . . ? O3 C46 O1 122.8(5) . . ? O3 C46 O2 122.8(5) . . ? O1 C46 O2 114.4(5) . . ? O3 C46 Fe1 179.1(4) . . ? O1 C46 Fe1 56.6(3) . . ? O2 C46 Fe1 57.9(3) . . ? C1A B1 C1 7.4(13) . . ? C1A B1 C8 112.5(8) . . ? C1 B1 C8 107.9(10) . . ? C1A B1 C7 107.2(9) . . ? C1 B1 C7 114.5(9) . . ? C8 B1 C7 106.9(4) . . ? C1A B1 C9 109.7(11) . . ? C1 B1 C9 107.2(14) . . ? C8 B1 C9 111.0(4) . . ? C7 B1 C9 109.3(4) . . ? C2 C1 C6 114.5(11) . . ? C2 C1 B1 122.3(12) . . ? C6 C1 B1 123.2(13) . . ? C1 C2 C3 122.9(13) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C4 C3 C2 120.6(13) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 118.4(14) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 120.7(14) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 122.6(14) . . ? C1 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6A C1A C2A 116.0(10) . . ? C6A C1A B1 121.2(12) . . ? C2A C1A B1 122.4(10) . . ? C1A C2A C3A 121.1(11) . . ? C1A C2A H2A 119.5 . . ? C3A C2A H2A 119.5 . . ? C4A C3A C2A 121.4(12) . . ? C4A C3A H3A 119.3 . . ? C2A C3A H3A 119.3 . . ? C3A C4A C5A 118.6(12) . . ? C3A C4A H4A 120.7 . . ? C5A C4A H4A 120.7 . . ? C4A C5A C6A 120.6(12) . . ? C4A C5A H5A 119.7 . . ? C6A C5A H5A 119.7 . . ? C1A C6A C5A 122.1(11) . . ? C1A C6A H6A 118.9 . . ? C5A C6A H6A 118.9 . . ? B1 C7 P1 111.5(3) . . ? B1 C7 H7A 109.3 . . ? P1 C7 H7A 109.3 . . ? B1 C7 H7B 109.3 . . ? P1 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 P1 C10 105.1(2) . . ? C7 P1 C16 107.8(2) . . ? C10 P1 C16 100.0(2) . . ? C7 P1 Fe1 117.32(17) . . ? C10 P1 Fe1 115.77(17) . . ? C16 P1 Fe1 109.24(16) . . ? C15 C10 C11 116.5(5) . . ? C15 C10 P1 123.1(4) . . ? C11 C10 P1 120.4(4) . . ? C12 C11 C10 120.5(5) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.9(5) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C12 C13 C14 118.7(5) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C13 C14 C15 119.3(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 123.0(5) . . ? C10 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C21 C16 C17 119.1(4) . . ? C21 C16 P1 117.6(4) . . ? C17 C16 P1 123.2(4) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.1(5) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 119.7(5) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 120.6(5) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? B1 C8 P2 115.1(3) . . ? B1 C8 H8A 108.5 . . ? P2 C8 H8A 108.5 . . ? B1 C8 H8B 108.5 . . ? P2 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 P2 C22 106.8(2) . . ? C8 P2 C28 106.6(2) . . ? C22 P2 C28 99.7(2) . . ? C8 P2 Fe1 115.65(17) . . ? C22 P2 Fe1 108.91(17) . . ? C28 P2 Fe1 117.48(17) . . ? C27 C22 C23 117.8(4) . . ? C27 C22 P2 124.8(4) . . ? C23 C22 P2 117.4(4) . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.9(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.5(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 120.9(5) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C33 C28 C29 117.1(5) . . ? C33 C28 P2 123.4(4) . . ? C29 C28 P2 119.5(4) . . ? C30 C29 C28 120.8(5) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 120.4(5) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 119.6(5) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 122.0(5) . . ? C32 C33 H33 119.0 . . ? C28 C33 H33 119.0 . . ? B1 C9 P3 113.8(3) . . ? B1 C9 H9A 108.8 . . ? P3 C9 H9A 108.8 . . ? B1 C9 H9B 108.8 . . ? P3 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 P3 C40 108.4(2) . . ? C9 P3 C34 106.5(2) . . ? C40 P3 C34 99.3(2) . . ? C9 P3 Fe1 113.58(16) . . ? C40 P3 Fe1 114.08(16) . . ? C34 P3 Fe1 113.79(16) . . ? C39 C34 C35 118.0(4) . . ? C39 C34 P3 123.1(4) . . ? C35 C34 P3 118.9(4) . . ? C36 C35 C34 120.9(5) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 120.9(5) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 119.0(5) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C37 C38 C39 120.3(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C34 C39 C38 120.9(5) . . ? C34 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C41 C40 C45 116.7(5) . . ? C41 C40 P3 123.2(4) . . ? C45 C40 P3 120.0(4) . . ? C40 C41 C42 121.7(5) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C43 C42 C41 120.4(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.4(5) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C45 120.2(5) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 121.6(5) . . ? C44 C45 H45 119.2 . . ? C40 C45 H45 119.2 . . ? C47 B2 C55 104.5(4) . . ? C47 B2 C53 110.1(4) . . ? C55 B2 C53 111.7(4) . . ? C47 B2 C54 109.8(5) . . ? C55 B2 C54 111.7(4) . . ? C53 B2 C54 109.0(4) . . ? C52 C47 C48 113.7(6) . . ? C52 C47 B2 125.2(6) . . ? C48 C47 B2 120.7(5) . . ? C49 C48 C47 123.6(6) . . ? C49 C48 H48 118.2 . . ? C47 C48 H48 118.2 . . ? C50 C49 C48 118.4(7) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C51 C50 C49 120.2(7) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 119.7(7) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C47 C52 C51 124.4(7) . . ? C47 C52 H52 117.8 . . ? C51 C52 H52 117.8 . . ? B2 C53 P4 117.9(3) . . ? B2 C53 H53A 107.8 . . ? P4 C53 H53A 107.8 . . ? B2 C53 H53B 107.8 . . ? P4 C53 H53B 107.8 . . ? H53A C53 H53B 107.2 . . ? C53 P4 C62 109.5(2) . . ? C53 P4 C56 105.7(2) . . ? C62 P4 C56 102.5(2) . . ? C53 P4 Fe2 108.24(16) . . ? C62 P4 Fe2 108.54(17) . . ? C56 P4 Fe2 121.86(17) . . ? C61 C56 C57 118.8(5) . . ? C61 C56 P4 120.6(4) . . ? C57 C56 P4 120.6(4) . . ? C58 C57 C56 120.4(5) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C57 C58 C59 120.6(5) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C58 C59 C60 119.5(5) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C61 C60 C59 120.0(5) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C56 120.7(5) . . ? C60 C61 H61 119.7 . . ? C56 C61 H61 119.7 . . ? C63 C62 C67 116.9(5) . . ? C63 C62 P4 124.4(4) . . ? C67 C62 P4 118.5(4) . . ? C64 C63 C62 121.9(5) . . ? C64 C63 H63 119.0 . . ? C62 C63 H63 119.0 . . ? C65 C64 C63 119.6(6) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C66 C65 C64 119.3(6) . . ? C66 C65 H65 120.4 . . ? C64 C65 H65 120.4 . . ? C67 C66 C65 120.9(6) . . ? C67 C66 H66 119.6 . . ? C65 C66 H66 119.6 . . ? C66 C67 C62 121.4(5) . . ? C66 C67 H67 119.3 . . ? C62 C67 H67 119.3 . . ? B2 C54 P5 117.0(4) . . ? B2 C54 H54A 108.0 . . ? P5 C54 H54A 108.0 . . ? B2 C54 H54B 108.0 . . ? P5 C54 H54B 108.0 . . ? H54A C54 H54B 107.3 . . ? C54 P5 C68 107.1(2) . . ? C54 P5 C74 108.6(2) . . ? C68 P5 C74 102.1(2) . . ? C54 P5 Fe2 108.80(17) . . ? C68 P5 Fe2 120.29(18) . . ? C74 P5 Fe2 109.36(18) . . ? C73 C68 C69 118.0(5) . . ? C73 C68 P5 122.2(4) . . ? C69 C68 P5 119.8(4) . . ? C70 C69 C68 120.4(6) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C71 C70 C69 120.2(6) . . ? C71 C70 H70 119.9 . . ? C69 C70 H70 119.9 . . ? C70 C71 C72 120.3(6) . . ? C70 C71 H71 119.9 . . ? C72 C71 H71 119.9 . . ? C73 C72 C71 118.9(6) . . ? C73 C72 H72 120.6 . . ? C71 C72 H72 120.6 . . ? C68 C73 C72 122.2(6) . . ? C68 C73 H73 118.9 . . ? C72 C73 H73 118.9 . . ? C75 C74 C79 119.5(5) . . ? C75 C74 P5 118.0(4) . . ? C79 C74 P5 122.4(4) . . ? C74 C75 C76 121.6(5) . . ? C74 C75 H75 119.2 . . ? C76 C75 H75 119.2 . . ? C77 C76 C75 119.2(6) . . ? C77 C76 H76 120.4 . . ? C75 C76 H76 120.4 . . ? C78 C77 C76 120.0(6) . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 120.9(5) . . ? C77 C78 H78 119.5 . . ? C79 C78 H78 119.5 . . ? C74 C79 C78 118.8(5) . . ? C74 C79 H79 120.6 . . ? C78 C79 H79 120.6 . . ? B2 C55 P6 121.1(4) . . ? B2 C55 H55A 107.1 . . ? P6 C55 H55A 107.1 . . ? B2 C55 H55B 107.1 . . ? P6 C55 H55B 107.1 . . ? H55A C55 H55B 106.8 . . ? C55 P6 C86 107.9(2) . . ? C55 P6 C80 106.2(2) . . ? C86 P6 C80 98.8(2) . . ? C55 P6 Fe2 105.54(17) . . ? C86 P6 Fe2 125.40(17) . . ? C80 P6 Fe2 111.57(16) . . ? C81 C80 C85 118.6(4) . . ? C81 C80 P6 120.7(4) . . ? C85 C80 P6 120.5(4) . . ? C82 C81 C80 120.6(5) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C83 C82 C81 120.5(5) . . ? C83 C82 H82 119.7 . . ? C81 C82 H82 119.7 . . ? C82 C83 C84 119.5(5) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? C83 C84 C85 120.8(5) . . ? C83 C84 H84 119.6 . . ? C85 C84 H84 119.6 . . ? C84 C85 C80 120.0(5) . . ? C84 C85 H85 120.0 . . ? C80 C85 H85 120.0 . . ? C87 C86 C91 117.4(5) . . ? C87 C86 P6 119.1(4) . . ? C91 C86 P6 123.1(4) . . ? C86 C87 C88 123.8(6) . . ? C86 C87 H87 118.1 . . ? C88 C87 H87 118.1 . . ? C87 C88 C89 119.0(6) . . ? C87 C88 H88 120.5 . . ? C89 C88 H88 120.5 . . ? C90 C89 C88 118.6(6) . . ? C90 C89 H89 120.7 . . ? C88 C89 H89 120.7 . . ? C89 C90 C91 121.5(6) . . ? C89 C90 H90 119.2 . . ? C91 C90 H90 119.2 . . ? C86 C91 C90 119.7(6) . . ? C86 C91 H91 120.2 . . ? C90 C91 H91 120.2 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 50.44 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.972 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.062 # start Validation Reply Form _vrf_PLAT029_complex5 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.900 RESPONSE: The dataset is 99.7 % complete to theta = 25.24. The missing high angle data may be due to the square detector employed. ; _vrf_PLAT222_complex5 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: The structure was highly disordered, and the dataset was modelled with the use of free variables and appropriate restraints. The dataset was not strong enough to permit for location of all of the disordered atoms, resulting in some large U-values. ; _vrf_PLAT410_complex5 ; PROBLEM: Short Intra H...H Contact H1A4 .. H2A2 .. 1.52 Ang. RESPONSE: All close contacts, both inter and intramolecular, involve at least one partner from a minor component of a disordered moiety (and in most instances, both partners are from disordered components). While it is conceivable that more components of the structures are disordered and parameterization of these disordered components would remove the close contacts, the data at hand did not allow for further modeling of the disorder. ; _vrf_PLAT761_complex5 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: ; _vrf_PLAT762_complex5 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ... ; _vrf_PLAT029_complex6 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.896 RESPONSE: The dataset is 99.6 % complete to theta = 23.01. The missing high angle data may be due to the square detector employed. ; _vrf_PLAT241_complex6 ; PROBLEM: Check High Ueq as Compared to Neighbors for C4_1 RESPONSE: This is due to disorder within the molecule. The data at hand did not allow for modelling of the disorder. ; _vrf_PLAT411_complex6 ; PROBLEM: Short Inter H...H Contact H4A_1 .. H6B_31 .. 1.73 Ang. RESPONSE: All close contacts, both inter and intramolecular, involve at least one partner from a minor component of a disordered moiety (and in most instances, both partners are from disordered components). While it is conceivable that more components of the structures are disordered and parameterization of these disordered components would remove the close contacts, the data at hand did not allow for further modeling of the disorder. ; _vrf_PLAT761_complex6 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: ... ; _vrf_PLAT762_complex6 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ... ; _vrf_PLAT029_complex10 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.911 RESPONSE: The dataset is 97.4 % complete to theta = 25.24. The missing high angle data may be due to the square detector employed. ; _vrf_PLAT761_complex10 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: ... ; _vrf_PLAT762_complex10 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ... ; _vrf_PLAT761_complex12 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: ... ; _vrf_PLAT762_complex12 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: ... ; _vrf_PLAT029_complex14 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.937 RESPONSE: The dataset is 99.9 % complete to theta = 27.0. The missing high angle data may be due to the square detector employed. ; _vrf_DENSD01_complex15 ; PROBLEM: The ratio of the submitted crystal density and that RESPONSE: The unit cell contains 8 highly disordered THF molecules. We were unable to satisfactorily model this disorder and the program SQUEEZE was used to deal with the disorder. Details can be found at the end of the "_refine_special_details" for complex15. ; _vrf_THETM01_complex15 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Crystals of complex 15 were small and did not diffract well. We were unable to grow better crystals from different solvent systems/techniques. Despite the poor quality, connectivity could be established. ; _vrf_PLAT023_complex15 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 50.44 Deg. RESPONSE: Crystals of complex 15 were small and did not diffract well. We were unable to grow better crystals from different solvent systems/techniques. Despite the poor quality, connectivity could be established. ; _vrf_PLAT029_complex15 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.938 RESPONSE: The dataset is 99.9 % complete to theta = 27.0. ; _vrf_PLAT046_complex15 ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.108 RESPONSE: The unit cell contains 8 highly disordered THF molecules. We were unable to satisfactorily model this disorder and the program SQUEEZE was used to deal with the disorder. Details can be found at the end of the "_refine_special_details" for complex15. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 937865'